Pyridine → 1-methyl-7-chloro-3-dipropylacetoxy-5-phenyl-1,3-dihydro-2H-1,4-benzodiazepine-2-one

HRID 443793

반응식

HRID 443793 반응식
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][C:11]([Cl:13])=[CH:12][C:7]=2[C:6]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:5][CH:4]([OH:20])[C:3]1=[O:21].N1C=CC=CC=1.[CH2:28]([CH:31]([CH2:35][CH2:36][CH3:37])[C:32](Cl)=[O:33])[CH2:29][CH3:30]>CN(C)C=O>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][C:11]([Cl:13])=[CH:12][C:7]=2[C:6]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:5][CH:4]([O:20][C:32](=[O:33])[CH:31]([CH2:35][CH2:36][CH3:37])[CH2:28][CH2:29][CH3:30])[C:3]1=[O:21]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 5391TemazepamHCID 762402-Propylvaleryl chloride

생성물 1

HCID 234655641-methyl-7-chloro-3-dipropylacetoxy-5-phenyl-1,3-dihydro-2H-1,4-benzodiazepine-2-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 15 g of 1-methyl-7-chloro-3-hydroxy-5-phenyl-1,3-dihydro-2H-1,4-benzodiazepine-2-one (Temazepam) and 5 g of absolute pyridine is cooled in 40 ml of freshly distilled dimethyl formamide to -5° and is mixed drop by drop with 10.5 g of dipropyl acetic acid chloride with the exclusion of atmospheric moisture. The mixture is stirred for an additional 4 hours at -5° and is allowed to stand over night at 0°, and then the mixture is poured on ice. The separated oil crystallizes while rubbed on with ethanol. By recrystallization from petroleum ether or isopropanol using activated charcoal, one will obtain the 1-methyl-7-chloro-3-dipropylacetoxy-5-phenyl-1,3-dihydro-2H-1,4-benzodiazepine-2-one as a colorless powder with a melting point of 134°-136°.

후처리

  1. waitto stand over night at 0°
  2. additionthe mixture is poured on ice
  3. customThe separated oil crystallizes
  4. customBy recrystallization from petroleum ether or isopropanol using activated charcoal, one

출처 및 근거

ORD 기록
ord-b58383cd293c40228718e3d99a150283
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04261987

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