LCMS was performed on an Agilent 1260
Infinity II system. The photodiode array detector HS (215 nm or unless
otherwise stated) coupled directly to an electrospray ionization source
and an Agilent 6120 single quadrupole mass analyzer. Standard RP-HPLC
analysis was performed at 40 °C using an Agilent InfinityLab
Poroshell 120 EC-C8 3.0 × 50 mm 2.7 μm column, fitted with
an InfinityLab Poroshell 120 EC-C8 3.0 × 5 mm 2.7 μm guard
column. The column eluted with a gradient of 0–60% ACN in 0.05%
aqueous TFA over 9 min at a flow rate of 0.5 mL/min. Mass spectra
were obtained in the positive mode with a scan range of 2–2000 m/z. Buffer A was 0.05% v/v TFA in milli Q water, and buffer B was 0.05% v/v TFA in acetonitrile.
Identities of final products
were confirmed by high-resolution mass spectrometry (HRMS) spectra,
obtained using an Agilent MS Q-TOF (model G6545XT) using the (+)-ion
mode with a Dual AJS ESI ion source.
Analytical reverse-phase
HPLC was performed using an Agilent 1200
series HPLC system, fitted with an Eclipse XD8-C8 4.6 Å, 5 μm
column. Buffer A was 0.1% v/v TFA in milli Q
water, and buffer B was 0.08% v/v TFA in acetonitrile.
The column eluted with a gradient of 0–60% ACN in 0.08% aqueous
TFA over 10 min at a flow rate of 1 mL/min.
Infinity II system. The photodiode array detector HS (215 nm or unless
otherwise stated) coupled directly to an electrospray ionization source
and an Agilent 6120 single quadrupole mass analyzer. Standard RP-HPLC
analysis was performed at 40 °C using an Agilent InfinityLab
Poroshell 120 EC-C8 3.0 × 50 mm 2.7 μm column, fitted with
an InfinityLab Poroshell 120 EC-C8 3.0 × 5 mm 2.7 μm guard
column. The column eluted with a gradient of 0–60% ACN in 0.05%
aqueous TFA over 9 min at a flow rate of 0.5 mL/min. Mass spectra
were obtained in the positive mode with a scan range of 2–2000 m/z. Buffer A was 0.05% v/v TFA in milli Q water, and buffer B was 0.05% v/v TFA in acetonitrile.
Identities of final products
were confirmed by high-resolution mass spectrometry (HRMS) spectra,
obtained using an Agilent MS Q-TOF (model G6545XT) using the (+)-ion
mode with a Dual AJS ESI ion source.
Analytical reverse-phase
HPLC was performed using an Agilent 1200
series HPLC system, fitted with an Eclipse XD8-C8 4.6 Å, 5 μm
column. Buffer A was 0.1% v/v TFA in milli Q
water, and buffer B was 0.08% v/v TFA in acetonitrile.
The column eluted with a gradient of 0–60% ACN in 0.08% aqueous
TFA over 10 min at a flow rate of 1 mL/min.