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Potassium Cyanide → cyclobutylmethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate

HRID 1154452
ノート
印刷プレビュー

反応式

HRID 1154452 の反応式
[Cl: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]1CC[CH2:28]1.[C-]#N.[K+]>C(O)C>[Cl: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[CH2:28][CH2:27][CH2:26]3)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 9032Potassium CyanideHCID 78130CyclobutylcarbinolHCID 53890667ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]-benzodiazepine-1-carboxylate

生成物 1

HCID 54120508cyclobutylmethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

10.35 g (0.03 mmol) of ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate, 25 ml of hydroxymethylcyclobutane and 0.5 g of powdered potassium cyanide are heated to 165° for 2 hours, the ethanol formed being distilled off continuously. The mixture is subsequently evaporated in vacuo, the residue is taken up in chloroform, the chloroform solution is washed three times with water, dried over magnesium sulphate and evaporated. By recrystallization of the resulting material from ethyl acetate there is obtained cyclobutylmethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 204°-205°.

後処理

  1. distillationbeing distilled off continuously
  2. customThe mixture is subsequently evaporated in vacuo
  3. washthe chloroform solution is washed three times with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customBy recrystallization of the resulting material from ethyl acetate

出典と根拠

ORDレコード
ord-2d743c1bcb1d4a31aeebff779f98ef0b
出典データセット
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04489003

反応ノート

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