The reaction progress was monitored using thin-layer chromatography (TLC) on silica gel 60 F254 (0.25 mm, Merck, Darmstadt, Germany). Column chromatography was performed using silica gel 60 (0.04–0.063 mm, Merck). Melting points were determined using a Yanaco (Tokyo, Japan) micro-melting-point apparatus without correction. HPLC was performed using an EYELA Preparative LC system [VSP-3050 pump, UV-9000 spectrometric detector, LiChrosorb RP-18 column (10 μm, 25 mm × 300 mm)] (Tokyo Rikakikai Co. Ltd., Tokyo, Japan) and a Shimadzu LC system [LC-6 AD pump, SPD-20A UV spectrometric detector, Mightysil RP-18 column (5 μm, 20 mm × 250 mm)] (Kyoto, Japan). The NMR spectra were recorded with a JEOL JNM-LA400 spectrometer (Tokyo, Japan). The chemical shifts were expressed in ppm, downfield from TMS. The mass spectra were collected using a JEOL JMS-SX102A mass spectrometer (Tokyo, Japan).
Jms sx102a mass spectrometer
Manufactured by JEOL
Sourced in Japan
The JMS-SX102A is a high-performance mass spectrometer manufactured by JEOL. It is designed to accurately analyze the molecular composition of various samples. The instrument utilizes advanced ion detection technology to provide precise and reliable measurement of molecular weights and fragmentation patterns.
Automatically generated - may contain errors
Lab products found in correlation
Jnm la400 spectrometer, by JEOL (2 mentions)
Silica gel 60, by Merck Group (2 mentions)
Lc 6ad pump, by Shimadzu (2 mentions)
Spd m20a uv vis detector, by Shimadzu (1 mentions)
Lc 20ad pump, by Shimadzu (1 mentions)
Ecs 400, by JEOL (1 mentions)
Cosmosil 5c18 ms 2, by Nacalai Tesque (1 mentions)
Jnm eca600, by JEOL (1 mentions)
Silica gel 60, by Kanto Chemical (1 mentions)
Sil 20a auto injector, by Shimadzu (1 mentions)
Silica gel 60 f254, by Merck Group (1 mentions)
Spd 20a, by Shimadzu (1 mentions)
Jes x320, by JEOL (1 mentions)
Avance 500, by Bruker (1 mentions)
Silica gel 60n, by Kanto Chemical (1 mentions)
Ap 224x, by Shimadzu (1 mentions)
Jnm eca 600 ft nmr spectrometer, by JEOL (1 mentions)
Pu 980, by Jasco (1 mentions)
P 1010 polarimeter, by Jasco (1 mentions)
Uv 970, by Jasco (1 mentions)
7 protocols using jms sx102a mass spectrometer
1
Characterization of Organic Compounds
2
Spectroscopic Analysis of Chemical Compounds
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Specific rotations were obtained by using a JASCO P-2200 digital polarimeter (l = 5 cm). ECD spectroscopy was recorded using a JASCO J-1500 spectrometer. FAB-MS and HR-FAB-MS were recorded by using a JEOL JMS-SX 102 A mass spectrometer. 1 H NMR spectroscopy was recorded on JEOL ECS400 (400 MHz) and JNM-ECA 600 (600 MHz) spectrometers. 13 C NMR spectroscopy was recorded on a JNM-ECA 600 (150 MHz) spectrometer. 2D-NMR experiments were carried out on a JEOL JNM-ECA 600 (600 MHz) spectrometer.
Normal phase silica gel column chromatography was carried out using Silica gel 60 (Kanto Chemical Co., Inc. 63–210 mesh), and reversed phase silica gel column chromatography was carried out using C18-OPN (Nacalai Tesque Co., Inc. 140 μm). High-performance liquid chromatography (HPLC) was performed using a Shimadzu SPD-M20A UV–vis detector, Shimadzu LC-20AD pump, and Shimadzu SIL-20 A auto-injector. COSMOSIL 5C18-MS-II (Nacalai Tesque Co., Inc. 250 × 4.6 mm i.d., 250 × 10 mm i.d., and 250 × 20 mm i.d.) columns were used for analytical and preparative work.
Normal phase silica gel column chromatography was carried out using Silica gel 60 (Kanto Chemical Co., Inc. 63–210 mesh), and reversed phase silica gel column chromatography was carried out using C18-OPN (Nacalai Tesque Co., Inc. 140 μm). High-performance liquid chromatography (HPLC) was performed using a Shimadzu SPD-M20A UV–vis detector, Shimadzu LC-20AD pump, and Shimadzu SIL-20 A auto-injector. COSMOSIL 5C18-MS-II (Nacalai Tesque Co., Inc. 250 × 4.6 mm i.d., 250 × 10 mm i.d., and 250 × 20 mm i.d.) columns were used for analytical and preparative work.
3
Chromatographic and Spectroscopic Characterization of Organic Compounds
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The reaction progress was monitored using thin-layer chromatography (TLC) on silica gel 60 F254 (0.25 mm, Merck, Darmstadt, Germany). Column chromatography was performed using silica gel 60 (0.04–0.063 mm, Merck). Melting points were determined using a Yanaco (Tokyo, Japan) micro-melting point apparatus without correction. The LC system used was equipped with an LC-6 AD pump (Shimadzu, Kyoto, Japan), a UVDEC-100 V spectrometric detector (JASCO, Tokyo, Japan), a YRD-880 IR detector (Shimamura Tech. Co. Ltd., Tokyo, Japan), or a SPD-20A (Shimadzu), and a Capcell pack RP-18 column (Shiseido, Tokyo, Japan). NMR spectra were recorded with a JEOL JNM-LA400 spectrometer (Tokyo, Japan). The chemical shifts were expressed as ppm downfield from TMS. The mass spectra were measured on a JEOL JMS-SX102A mass spectrometer. The ESR spectra were collected on a JEOL JES-X320.
4
Reductive Amination of 3-Phenoxybenzaldehyde
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To a solution of 3-phenoxybenzaldehyde (1 equivalent) in dichloromethane, piperazin-1-yl (thiophen-2-yl) methanone hydrochloride (1.1 equivalent) and sodium acetoxyborohydride (1.2 equivalent) were added. The reaction mixture was stirred at room temperature. After stirring overnight, the reaction was quenched by the addition of water and was then extracted with chloromethane. The organic layer was washed with brine and was dried with anhydrous Na 2 SO 4 . The organic solvent was evaporated under reduced pressure to obtain the crude product. The reaction was carried out under an argon atmosphere. The compound was purified by silica gel column chromatography (Kanto Chemical Silica Gel 60N). NMR spectra were recorded on Bruker Avance 500 (Bruker) in CDCl 3 (Tetramethylsilane for 1H, δ = 0) or CDCl 3 (for 13C, δ = 77.0) was used as an internal standard. Mass spectra were obtained with a JEOL JMS-SX102A mass spectrometer (JEOL). Yield: 46%. 1
5
Characterization of [C4mpyr][OH] in DMSO
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[C4mpyr][OH] aqueous solution was diluted in DMSO-d6 with tetramethylsilane as reference. It was characterized by 1H NMR spectroscopy on a Bruker AVANCE III HD NanoBay 400 MHz NMR spectrometer from Bruker Corporation (Billerica, MA, USA) at 25 °C. Mass spectra were measured on a JEOL JMS-SX 102A mass spectrometer from JEOL Ltd. (Akishima-shi, Tokyo, Japan). The water content was determined in triplicates through Karl Fischer titration using a Kyoto Electronics Manufacturing MKH-710M titrator from Kyoto Electronics Manufacturing Co., Ltd. (Minami-ku, Kyoto, Japan), and the average was used. The titration performance was regularly checked with KEMAQUA Water Standard 10 from Kyoto Electronics Manufacturing Co., Ltd. (Minami-ku, Kyoto, Japan) containing 1% water to adjust the titration factor. Throughout the experiments, a Shimadzu AP 224X from Shimadzu Corporation (Nakagyo-ku, Kyoto, Japan) weighing scale (d = 0.1 mg) was used.
6
Characterization of [C4mpyr][OH] by NMR and Mass Spectrometry
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[C4mpyr][OH] was characterized by 1H NMR spectroscopy on a Bruker AVANCE III HD Nano Boy 400 MHz NMR spectrometer at room temperature. Mass spectra were measured on a Jeol JMS-SX 102A mass spectrometer. Water contents were determined in triplicates though Karl-Fischer titration using a Kyoto Electronics Manufacturing MKH-710M titrator, and the average was used. The titration performance was regularly checked with KEMAQUA Water Standard 10 containing 1% water to adjust the titration factor. Throughout the experiments, a Shimadzu AP 224X weighing scale (d = 0.1 mg) was used.
7
Analytical Characterization of Organic Compounds
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Column chromatography was conducted on an FMI pump system (Yamazen) with a column of Merck silica gel 60 (230-400 mesh, ASTM). Analytical thin-layer chromatography (TLC) and preparative TLC were performed using plates precoated with Merck silica gel 60 F 254 (thicknesses of 0.25 and 0.50 mm, respectively). Analytical high-performance liquid chromatography (HPLC) was carried out on a Jasco PU-980 equipped with a Jasco UV-970 intelligent UV/Vis detector (280 nm) and Spectra Manager (ver.1.53) using a reversed-phase column (TSK-GEL ODS-80Ts, 250 9 4.6 mm i.d., Tosoh). Preparative HPLC was done using the same system with a different column size (300 9 7.8 mm i.d.). Chiral HPLC was performed on a Jasco PU2089 with Jasco OR-990 using chiral OD-H (250 9 4.6 mm i.d., Daisel). Optical rotation was recorded on a Jasco P-1010 polarimeter. 1 H and 13 C nuclear magnetic resonance (NMR) spectra and two-dimensional NMR spectra were obtained on a JEOL JNM ECA 600 FT-NMR spectrometer (600 MHz) using tetramethylsilane as an internal standard. Electron-impact (EI, 70 eV) and fast-atom bombardment (FAB) mass spectrometry (MS) were performed using a JEOL JMS-SX102A mass spectrometer. High-resolution time of flight mass spectrometry (HRTOFMS) was performed with a Waters Xevo G2-XS.
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