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Ammonia → 6-(2-chlorophenyl)-1,8-dichloro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide

HRID 261705
ノート
印刷プレビュー

反応式

HRID 261705 の反応式
C[O:2][C:3]([C:5]1[N:6]=[C:7]([Cl:27])[N:8]2[C:14]3[CH:15]=[CH:16][C:17]([Cl:19])=[CH:18][C:13]=3[C:12]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[Cl:26])=[N:11][CH2:10][C:9]=12)=O.[NH3:28].[K+].[Br-]>CO.C(Cl)Cl>[Cl:26][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=1[C:12]1[C:13]2[CH:18]=[C:17]([Cl:19])[CH:16]=[CH:15][C:14]=2[N:8]2[C:7]([Cl:27])=[N:6][C:5]([C:3]([NH2:28])=[O:2])=[C:9]2[CH2:10][N:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 222AmmoniaHCID 253877Potassium BromideHCID 541351956-(2-chlorophenyl)-1,8-dichloro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid methyl ester

生成物 1

HCID 203945796-(2-chlorophenyl)-1,8-dichloro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

A mixture of 0.5 g (0.0012 mole) of 6-(2-chlorophenyl)-1,8-dichloro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid methyl ester and 20 ml of a 20% solution of ammonia in methanol was heated at 120°-125° in a steel bomb for 18 hrs. Evaporation of the solvent at reduced pressure gave an amorphous solid. The solid was dissolved in methylene chloride, washed with water, dried and evaporated at reduced pressure to give a tan, amorphous solid which crystallized when stirred with a small amount of boiling ether. Recrystallization from a solution of methanol and methylene chloride gave white crystals with mp 285°-288°. Uv λ 214 mμ (ε=44,300) sh 245 (26,500) sh 260 (16,400) sh 300 (600); ir (KBr) 3470, 3335 cm-1 (NH2) 1670 (CON).

後処理

  1. customEvaporation of the solvent at reduced pressure
  2. customgave an amorphous solid
  3. washwashed with water
  4. customdried
  5. customevaporated at reduced pressure
  6. customto give a tan, amorphous solid which
  7. customcrystallized when
  8. customRecrystallization from a solution of methanol and methylene chloride
  9. customgave white crystals with mp 285°-288°

出典と根拠

ORDレコード
ord-6280127298254546b4618c3169c0d4f9
出典データセット
uspto-grants-1979_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04166185

反応ノート

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