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Methanol → 1-(beta-Hydroxy-ethyl)-5-phenyl-7-chloro-1H-1,5-benzodiazepine-2,4-(3H,5H)-dione

HRID 1283338
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HRID 1283338 반응식
[C:1]1([N:7]2[C:13]3[CH:14]=[C:15]([Cl:18])[CH:16]=[CH:17][C:12]=3[NH:11][C:10](=[O:19])[CH2:9][C:8]2=[O:20])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.[CH2:23]1[O:25][CH2:24]1.[OH-].C([N+](C)(C)C)C1C=CC=CC=1>O>[OH:25][CH2:24][CH2:23][N:11]1[C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:13]=2[N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:8](=[O:20])[CH2:9][C:10]1=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 6354Ethylene OxideHCID 66854Benzyltrimethylammonium hydroxideHCID 89657Desmethylclobazam

생성물 1

HCID 215171751-(beta-Hydroxy-ethyl)-5-phenyl-7-chloro-1H-1,5-benzodiazepine-2,4-(3H,5H)-dione

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture consisting of 28.6 gm (0.1 mol) of 5-phenyl-7-chloro-1H-1,5-benzodiazepine-2,4-(3H,5H)-dione, 500 ml of methanol, 25 ml of water, 10-15 ml of ethyleneoxide and 1 ml of Triton B (methanolic 35% solution of benzyl trimethylammonium hydroxide) was stirred at room temperature for about eight hours. Thereafter, the clear solution formed thereby was evaporated, the residue was taken up in methylene chloride, and the resulting solution was extracted with water, dried and evaporated. The residue was recrystallized from ethanol, yielding 25.6 gm (78% of theory) of the colorless crystalline compound of the formula ##SPC6##

후처리

  1. customThereafter, the clear solution formed
  2. customthereby was evaporated
  3. extractionthe resulting solution was extracted with water
  4. customdried
  5. customevaporated
  6. customThe residue was recrystallized from ethanol
  7. customyielding 25.6 gm (78% of theory) of the colorless crystalline compound of the formula

출처 및 근거

ORD 기록
ord-52a45b361d134fbdbe957583f0861db4
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE028935

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