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Potassium Cyanide → HCID 54361250, 화합물

HRID 1154433
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HRID 1154433 반응식
[Br:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.O[CH2:26][CH:27]1CC1.[C-]#N.[K+]>>[Br:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18][CH2:19][CH:20]3[CH2:27][CH2:26]3)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 9032Potassium CyanideHCID 75644CyclopropanemethanolHCID 54197869HCID 54197869, 화합물

생성물 1

HCID 54361250HCID 54361250, 화합물

실험 절차

A mixture of 12 g (31 mmol) of ethyl (S)-8-bromo-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate, 60 ml (750 mmol) of hydroxymethyl-cyclopropane and 500 mg of powdered potassium cyanide is stirred at 135° for 1.5 hours, the alcohol being simultaneously distilled off over a Hickmann headpiece and a 15 cm Vigreux column. The mixture is evaporated to dryness, the residue is taken up in chloroform, washed with water, dried over magnesium sulphate and evaporated. By recrystallization from ethyl acetate there is obtained cyclopropylmethyl (S)-8-bromo-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 135°-136°.

후처리

  1. distillationthe alcohol being simultaneously distilled off over a Hickmann headpiece
  2. customThe mixture is evaporated to dryness
  3. washwashed with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customBy recrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-176b2081c2bb407588d492fa0a43e475
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04489003

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