反应详情

To a stirred solution of 3-tert-butoxycarbonyl-7-chloro-6-(4-hydroxymethyl-benzylthio)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (170 mg, 0.391 mmol) in anhydrous DCM under nitrogen, add methanesulfonyl chloride (33 μL, 0.426 mmol) and triethylamine (61 μL, 0.44 mmol) and continue stirring for 2 h. Dilute with water (5 mL) and extract three times with DCM. Wash the combined organic extracts with brine, dry over anhydrous Na2SO4, and concentrate in vacuo to obtain the desired intermediate that was used without purification.

1. extractionextract three times with DCM
2. washWash the combined organic extracts with brine
3. dry with materialdry over anhydrous Na2SO4
4. concentrationconcentrate in vacuo