Sodium Carbonate Decahydrate → 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde-3-oxime

HRID 67347

反応式

HRID 67347 の反応式
[OH2:1].O.O.O.O.O.O.O.O.O.C(=O)([O-])[O-].[Na+].[Na+].[F:17][C:18]1[CH:19]=[CH:20][C:21]2[N:27]3[CH:28]=[N:29][C:30]([CH:31]=O)=[C:26]3[CH2:25][N:24]([CH3:33])[C:23](=[O:34])[C:22]=2[CH:35]=1.Cl.[NH2:37]O>O>[F:17][C:18]1[CH:19]=[CH:20][C:21]2[N:27]3[CH:28]=[N:29][C:30]([CH:31]=[N:37][OH:1])=[C:26]3[CH2:25][N:24]([CH3:33])[C:23](=[O:34])[C:22]=2[CH:35]=1

参加物

5

反応物 3

HCID 151402Sodium Carbonate DecahydrateHCID 443297Hydroxyamine hydrochlorideHCID 198515378-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde

生成物 1

HCID 867382638-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde-3-oxime

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
70 °C

実験手順

A solution of 4.14 g (14.5 mmol) of sodium carbonate decahydrate in 20 ml of water is added dropwise to a mixture of 3.0 g (11.6 mmol) of 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde, 0.99 g (14.5 mmol) of hydroxylamine hydrochloride and 60 ml of water, the mixture is stirred at 70° C. for 1 hour, cooled in an ice-bath and the separated material is filtered off under suction and washed with water. The still moist substance is recrystallised from ethanol and yields 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxaldehyde-3-oxime of melting point 247°-250° C.

後処理

  1. temperaturecooled in an ice-bath
  2. filtrationthe separated material is filtered off under suction
  3. washwashed with water
  4. customThe still moist substance is recrystallised from ethanol

出典と根拠

ORDレコード
ord-b34504642d104a8f81a3e97c9d923afd
出典データセット
uspto-grants-1982_08
特許番号
US04346031

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