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Hydrochloric Acid → (S)-8-bromo-9-oxo-12,12a-dihydro-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepine-1-carboxylic acid

HRID 1378163
ノート
印刷プレビュー

反応式

HRID 1378163 の反応式
[Br:1][C:2]1[C:7]2[C:8](=[O:23])[N:9]3[CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18]CC)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].C(O)C.Cl>O>[Br:1][C:2]1[C:7]2[C:8](=[O:23])[N:9]3[CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([OH:18])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=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 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 53712300ethyl (S)-8-bromo-9-oxo-12,12a-dihydro-9H,11H-azeto [2,1-c]imidazo [1,5-a][1,4]benzodiazepine-1-carboxylate

生成物 1

HCID 22876624(S)-8-bromo-9-oxo-12,12a-dihydro-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]benzodiazepine-1-carboxylic acid収率 98.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

21.8 g (57.9 mmol) of ethyl (S)-8-bromo-9-oxo-12,12a-dihydro-9H,11H-azeto [2,1-c]imidazo [1,5-a][1,4]benzodiazepine-1-carboxylate were heated to reflux for 15 minutes with 17 ml of 4N sodium hydroxide solution and 200 ml of ethanol. 17 ml of 4N hydrochloric acid and 250 ml of water were added at room temperature. The alcohol was evaporated and the suspension was cooled to 0°. By suction filtration and drying the crystals there were obtained 19.8 g (98%) of (S)-8-bromo-9-oxo-12,12a-dihydro-9H,11H-azeto[2,1-c]imidazo[1,5-a][1,4]-benzodiazepine-1-carboxylic acid of m.p. 178°-180°.

後処理

  1. customThe alcohol was evaporated
  2. temperaturethe suspension was cooled to 0°
  3. filtrationBy suction filtration
  4. customdrying the crystals

出典と根拠

ORDレコード
ord-879239a3f2784c7c88be4c9eca986a79
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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