Ammonia → 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide

HRID 67485ノート

反応式

HRID 67485 の反応式
[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([O:19]CC)=O)=[C:4]2[CH2:3]1.[Cl-].[NH4+:23].N>CO>[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([NH2:23])=[O:19])=[C:4]2[CH2:3]1

参加物

5

反応物 3

HCID 222AmmoniaHCID 25517Ammonium ChlorideHCID 127597Ro 14-7437

生成物 1

HCID 205153215,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
120 °C

実験手順

A mixture of 10.0 g of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate, 200 ml of methanol, 0.5 g of ammonium chloride and 30 g of ammonia (100%) is stirred in an autoclave under nitrogen (40 bar) at a temperature of 120° C. for 12 hours. After cooling and discharging the over-pressure, the mixture is evaporated to dryness. After partition of the residue between methylene chloride and water, the organic phase is dried and evaporated. The residue is recrystallised from ethyl acetate, there being obtained 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide in the form of white crystals of melting point 274°-275° C.

後処理

  1. temperatureAfter cooling
  2. customthe mixture is evaporated to dryness
  3. customAfter partition of the residue between methylene chloride and water
  4. customthe organic phase is dried
  5. customevaporated
  6. customThe residue is recrystallised from ethyl acetate, there

出典と根拠

ORDレコード
ord-ea97190421b9439d8396e8017932bcd9
出典データセット
uspto-grants-1982_08
特許番号
US04346034

反応ノート

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