Hydrochloric Acid → HCID 21249960, 화합물

HRID 1531653노트

반응식

HRID 1531653 반응식
Cl.[BH4-].[Na+].[Br:4][C:5]1[C:6]([O:26][CH3:27])=[CH:7][C:8]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=3)=[N:13][N:12]=[C:11]([CH3:24])[CH2:10][C:9]=2[CH:25]=1>CO.O>[Br:4][C:5]1[C:6]([O:26][CH3:27])=[CH:7][C:8]2[C:14]([C:15]3[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=3)=[N:13][NH:12][CH:11]([CH3:24])[CH2:10][C:9]=2[CH:25]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 21249973HCID 21249973, 화합물

생성물 1

HCID 21249960HCID 21249960, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

3.5 ml (43.2 mmol) of concentrated hydrochloric acid is first added, and then over about 10 minutes, 1.80 g (47.5 mmol) of sodium borohydride is added in portions to a suspension of 1.4 g (3.6 mmol) of 7-bromo-4-methyl-8-methoxy-1-(4-nitrophenyl)-5H-2,3-benzodiazepine (Example 3, Step C) in 60 ml of methanol. The suspension is stirred for another hour, and then diluted with water (60 ml). The crystalline material is suctioned off and washed with 50% aqueous methanol (3×50 ml). The 7-bromo-4-methyl-8-methoxy-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine that is obtained as a crude product is further purified by suspension in 8 ml of hot ethanol. After suctioning-off, 1.23 g (88%) of chrome yellow crystals with a melting point of 172-174° C. is obtained.

후처리

  1. washwashed with 50% aqueous methanol (3×50 ml)

출처 및 근거

ORD 기록
ord-d3cd79cfa23c4dbaabf64448cfb7e33c
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06200970B1

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