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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 67296
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HRID 67296 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

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온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b766bb24bbaa4517a10f7e16d310989a
출처 데이터셋
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04346030

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