反应详情

Add phosphoryl chloride (1.47 mL, 2.43 g, 15.85 mmoles) to 7-chloro-2-methyl-5,10-dihydro-11H-pyrrolo[2,1-c][1,4]benzodiazepin-11-one (1.117 g, 4.53 mmoles) in DCM (50 mL) and stir at room temperature over a weekend. Add ice water to the reaction mixture then add DCM, separate the aqueous layer and wash the DCM layer with water and sodium hydrogen carbonate solution. Dry the DCM solution with MgSO4, filter and evaporate the solvent in vacuo to give 7,11-dichloro-2-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepine (1.167 g).

1. customAdd ice water to the reaction mixture then add DCM, separate the aqueous layer
2. washwash the DCM layer with water and sodium hydrogen carbonate solution
3. dry with materialDry the DCM solution with MgSO4
4. filtrationfilter
5. customevaporate the solvent in vacuo