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Hydroxyamine hydrochloride → 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamidoxime

HRID 1378012
ノート
印刷プレビュー

反応式

HRID 1378012 の反応式
Cl.[NH2:2][OH:3].[F:4][C:5]1[CH:6]=[CH:7][C:8]2[N:14]3[CH:15]=[N:16][C:17]([C:18]#[N:19])=[C:13]3[CH2:12][N:11]([CH3:20])[C:10](=[O:21])[C:9]=2[CH:22]=1.C[O-].[Na+].[Na]>CO>[F:4][C:5]1[CH:6]=[CH:7][C:8]2[N:14]3[CH:15]=[N:16][C:17]([C:18](=[N:2][OH:3])[NH2:19])=[C:13]3[CH2:12][N:11]([CH3:20])[C:10](=[O:21])[C:9]=2[CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 443297Hydroxyamine hydrochlorideHCID 5360545SodiumHCID 98815428-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrileHCID 10942334Sodium Methoxide

生成物 1

HCID 540046888-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamidoxime収率 67.4%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

6.2 g (89.2 mmol) of hydroxylamine hydrochloride and 16.3 g (63.6 mmol) of 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile were added in succession at room temperature under argon to a sodium methylate solution which had been prepared in the usual manner from 2.0 g (86.9 mmol) of sodium and 85 ml of methanol. The reaction mixture was stirred at room temperature for 24 hrs. and then cooled in an ice bath. The separated crystals were filtered off and triturated in 35 ml of water. The white crystals were filtered off and dried at 60° in a vacuum. There were obtained 12.4 g (67%) of 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamidoxime as white crystals of m.p. 249°-250° (dec.).

後処理

  1. temperatureand then cooled in an ice bath
  2. filtrationThe separated crystals were filtered off
  3. customtriturated in 35 ml of water
  4. filtrationThe white crystals were filtered off
  5. customdried at 60° in a vacuum

出典と根拠

ORDレコード
ord-2f7ea9a47b8e4b76b25483fab3cc81cf
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05665718

反応ノート

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