Sodium Hydroxide → 7-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

HRID 1606972

反応式

HRID 1606972 の反応式
[Cl:1][C:2]1[C:7]2[CH2:8][N:9]([CH3:23])[CH2:10][C:11]3[N:12]([C:13](=O)[NH:14][C:15]=3[C:16]#[C:17]C(O)(C)C)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-:24].[Na+]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]([CH3:23])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]#[CH:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 703945457-chloro-4,5-dihydro-3-(3-hydroxy-3-methyl-1-butynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepine-one

生成物 1

HCID 198515337-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

660 mg (2 mmol) of 7-chloro-4,5-dihydro-3-(3-hydroxy-3-methyl-1-butynyl)-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepine-one was heated to boiling under reflux overnight with 80 mg of sodium hydroxide in 10 ml of toluene. After evaporation of the solvent the residue was dissolved in methylene chloride and the solution was washed twice with water, dried over magnesium sulphate and evaporated. After recrystallization of the residue from ethyl acetate there was obtained 7-chloro-3-ethynyl-4,5-dihydro-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 200°-201°.

後処理

  1. customAfter evaporation of the solvent the residue
  2. dissolutionwas dissolved in methylene chloride
  3. washthe solution was washed twice with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated
  6. customAfter recrystallization of the residue from ethyl acetate

出典と根拠

ORDレコード
ord-b7cc5f1888334266a16039bfa0431e1d
出典データセット
uspto-grants-1989_09
特許番号
US04863920

関連ノート

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