Ethyl Acetate → Ro 14-7437

HRID 67368

反応式

HRID 67368 の反応式
[NH2:1][C:2](=[C:8]1CNC(=O)[C:11]2[CH:16]=[CH:17][CH:18]=[CH:19][C:10]=2[NH:9]1)[C:3]([O:5][CH2:6][CH3:7])=[O:4].C(O[CH:23]([O:27]CC)[N:24]([CH3:26])[CH3:25])C.[C:30](OCC)(=O)C>>[CH3:26][N:24]1[C:23](=[O:27])[C:19]2[CH:18]=[CH:17][CH:16]=[CH:11][C:10]=2[N:9]2[CH:30]=[N:1][C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[C:8]2[CH2:25]1

参加物

4

反応物 3

HCID 8857Ethyl AcetateHCID 70913Dimethylformamide diethylacetalHCID 70542724ethyl alpha-amino-1,3,4,5-tetrahydro-5-oxo-2H-1,4-benzodiazepin-2-ylidene-acetate

生成物 1

HCID 127597Ro 14-7437

実験手順

4.1 g of ethyl α-amino-1,3,4,5-tetrahydro-5-oxo-2H-1,4-benzodiazepin-2-ylidene-acetate are dissolved in 25 ml of ethyl acetate, treated with 3.1 ml (18.1 mmol) of N,N-dimethylformamide diethyl acetal and heated to boiling under reflux for 0.5 hour. After cooling, the separated material is filtered off under suction and recrystallised from ethanol. After chromatography of the mother liquor, there is obtained a second portion of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of the same purity; melting point 166°-168° C.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 0.5 hour
  3. temperatureAfter cooling
  4. filtrationthe separated material is filtered off under suction
  5. customrecrystallised from ethanol

出典と根拠

ORDレコード
ord-7179a83ad66b4a8b8fe1f5f7ae03e1f3
出典データセット
uspto-grants-1982_08
特許番号
US04346031

関連ノート

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