1,4-Dioxane hydrochloride → 1-(2-toluoylmethyl)-2-oxo-3-amino-5-pivaloyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine

HRID 1979296노트

반응식

HRID 1979296 반응식
Cl.O1CCOCC1.[C:8]1([CH3:43])[C:9]([C:14]([CH2:16][N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[N:21]([C:28](=[O:33])[C:29]([CH3:32])([CH3:31])[CH3:30])[CH2:20][CH:19]([NH:34]C(OC(C)(C)C)=O)[C:18]2=[O:42])=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=1>C(O)C>[C:8]1([CH3:43])[C:9]([C:14]([CH2:16][N:17]2[C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[N:21]([C:28](=[O:33])[C:29]([CH3:31])([CH3:32])[CH3:30])[CH2:20][CH:19]([NH2:34])[C:18]2=[O:42])=[O:15])=[CH:10][CH:11]=[CH:12][CH:13]=1

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 21201777HCID 21201777, 화합물

생성물 1

HCID 212016481-(2-toluoylmethyl)-2-oxo-3-amino-5-pivaloyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine수율 95.5%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

4N HCl-dioxane solution (5 ml) was added to 1-(2-toluoylmethyl)-2-oxo-3-tert-butoxycarbonylamino-5-pivaloyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (540 mg) in ethanol (5 ml), and the mixture was stirred at 50° C. for 30 minutes. The reaction mixture was concentrated under reduced pressure, and saturated aqueous sodium bicarbonate solution was added to the residue, followed by extraction with methylene chloride. The extract was dried over anhydrous sodium sulfate, to thereby obtain 411 mg of the titled compound.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and saturated aqueous sodium bicarbonate solution
  2. additionwas added to the residue
  3. extractionfollowed by extraction with methylene chloride
  4. dry with materialThe extract was dried over anhydrous sodium sulfate

출처 및 근거

ORD 기록
ord-34640dd01b5e4768b190d6a6e5e895f9
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06239131B1

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