Water → HCID 131723610, compound

Participants

Reaction Steps

To a suspension of 126 mg of diethyl [[4-[[[(4,5,6,7-tetrahydrothieno[3,2-c]pyridin-2-yl)carbonyl]amino]acetyl]-o-phenylen]dioxy]diacetate synthesized according to the method described in WO 9421599 in 3 ml of N,N-dimethylformamide was added 105 mg of 1-acetoxyethyl 4-nitrophenyl carbonate under stirring at room temperature, and the mixture was stirred at 40° C. for 20 hours. The reaction was poured into 3 ml of water, and extracted with 5 ml of ethyl acetate. The separated organic layer was dried over magnesium sulfate, and the solvent was removed by distillation. The residue thus obtained was purified by chromatography on an LH-20 column (chloroform:methanol=1:1) and a silica gel column (chloroform:acetone=8:1) to give the title compound (25.8 mg, 16%) as a free base.

Provenance & Evidence