Hydrogen Bromide → 3-amino-5-cycloheptyl-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one

3(R,S)-[(Benzyloxycarbonyl)amino]-5-cycloheptyl-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one (435 mg) was treated with a solution of 30% hydrogen bromide in glacial acetic add (10 ml) and stirred for 20 min at room temperature. The mixture was then added dropwise onto cold (0° C.) diethyl ether (50 ml). A white solid precipitated which was filtered off. The solid was treated with 10% sodium hydroxide solution (50 ml), then extracted with ethyl acetate (80 ml). The organic layer was separated, dried (Na2SO4) and evaporated to give crude 3(R,S)-amino-5-cycloheptyl-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one as a colourless oil.

1. additionadd (10 ml)
2. customA white solid precipitated which
3. filtrationwas filtered off
4. additionThe solid was treated with 10% sodium hydroxide solution (50 ml)
5. extractionextracted with ethyl acetate (80 ml)
6. customThe organic layer was separated
7. dry with materialdried (Na2SO4)
8. customevaporated

ORDレコード

ord-904098f8f4964111ae5f163e4a47d59a

出典データセット

uspto-grants-1996_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05556969