Potassium Carbonate → 2-oxo-3-tert-butoxycarbonylamino-5-(3-methyl-2-butenyl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine

HRID 1979393

반응식

HRID 1979393 반응식
[O:1]=[C:2]1[NH:8][C:7]2[CH:9]=[C:10]([CH3:13])[CH:11]=[CH:12][C:6]=2[NH:5][CH2:4][CH:3]1[NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16].Br[CH2:23][CH:24]=[C:25]([CH3:27])[CH3:26].C(=O)([O-])[O-].[K+].[K+]>CO>[O:1]=[C:2]1[NH:8][C:7]2[CH:9]=[C:10]([CH3:13])[CH:11]=[CH:12][C:6]=2[N:5]([CH2:23][CH:24]=[C:25]([CH3:27])[CH3:26])[CH2:4][CH:3]1[NH:14][C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 700922-Butene, 1-bromo-3-methyl-HCID 212015812-oxo-3-tert-butoxycarbonylamino-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine

생성물 1

HCID 212017442-oxo-3-tert-butoxycarbonylamino-5-(3-methyl-2-butenyl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine수율 75%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2-Oxo-3-tert-butoxycarbonylamino-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (2.00 g) obtained from Referential Example 7 was suspended in methanol (20 ml), 1-bromo-3-methyl-2-butene (1.18 g) and potassium carbonate (997 mg) were added, the mixture was stirred for 2 hours at room temperature. The reaction mixture was concentrated under reduced pressure, water (100 ml) was added, and extracted with methylene chloride. The organic layer was washed with saturated aqueous sodium bicarbonate, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure, to thereby obtain 1.85 g of the titled compound (Yield: 71.4%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, water (100 ml)
  2. additionwas added
  3. extractionextracted with methylene chloride
  4. washThe organic layer was washed with saturated aqueous sodium bicarbonate
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-13fa98f2606243f2b4a762e4abc7a153
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06239131B1

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