Potassium Hydroxide → 8-Chloro-6-(2-chlorophenyl)-1,2-dihydro-4H-imidazo[1,5-a] [1,4]benzodiazepin-1-thione-3-carboxylic acid

HRID 261695ノート

反応式

HRID 261695 の反応式
[OH-].[K+].C[O:4][C:5]([C:7]1[NH:8][C:9](=[S:29])[N:10]2[C:16]3[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:15]=3[C:14]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[Cl:28])=[N:13][CH2:12][C:11]=12)=[O:6]>CO>[Cl:21][C:19]1[CH:18]=[CH:17][C:16]2[N:10]3[C:9](=[S:29])[NH:8][C:7]([C:5]([OH:6])=[O:4])=[C:11]3[CH2:12][N:13]=[C:14]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[Cl:28])[C:15]=2[CH:20]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 54335518HCID 54335518、化合物

生成物 1

HCID 203945858-Chloro-6-(2-chlorophenyl)-1,2-dihydro-4H-imidazo[1,5-a] [1,4]benzodiazepin-1-thione-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 1.1 g (0.02 mole) of potassium hydroxide in 40 ml of methanol was treated with 2.1 g (0.005 mole) of 8-chloro-6-(2-chlorophenyl)-1,2-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-1-thione-3-carboxylic acid methyl ester in a beaker. The solution was boiled in a steambath for 15 min and then evaporated at reduced pressure at 50°-60°. An aqueous solution of the residue was acidified with cold 6 N aqueous hydrochloric acid adding ice to keep the mixture cold. The solid was collected by filtration, washed with water and air dried on the funnel overnight to yield crude end product. Recrystallization from ethanol gave light tan crystals with mp 277°-280° (dec).

後処理

  1. customevaporated at reduced pressure at 50°-60°
  2. additionadding ice
  3. filtrationThe solid was collected by filtration
  4. washwashed with water and air
  5. customdried on the funnel overnight
  6. customto yield crude end product
  7. customRecrystallization from ethanol
  8. customgave light tan crystals with mp 277°-280° (dec)

出典と根拠

ORDレコード
ord-d431c64ea52a4e88aa10210e8f1fe97e
出典データセット
uspto-grants-1979_08
特許番号
US04166185

反応ノート

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