Ethyl Acetate → HCID 10403166, 화합물

HRID 1755630노트

반응식

HRID 1755630 반응식
[Br:1]Br.[C:3]([N:7]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][CH:17]=[CH:18][C:11]=2[NH:10][C:9](=[O:19])[CH2:8]1)([CH3:6])([CH3:5])[CH3:4].C([O-])(=O)C.[Na+].C(OCC)(=O)C>C(O)(=O)C>[Br:1][C:16]1[CH:17]=[CH:18][C:11]2[NH:10][C:9](=[O:19])[CH2:8][N:7]([C:3]([CH3:6])([CH3:4])[CH3:5])[C:13](=[O:14])[C:12]=2[CH:15]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 24408BromineHCID 517045Sodium AcetateHCID 100826661H-1,4-Benzodiazepine-2,5-dione, 4-(1,1-dimethylethyl)-3,4-dihydro-

생성물 1

HCID 10403166HCID 10403166, 화합물수율 64.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Bromine (1.72 g, 10.8 mmol) is added to a mixture of 4-tert-butyl-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione (1.0 g, 4.3 mmol) and sodium acetate (0.39 g, 4.8 mmol) in acetic acid. The reaction mixture is stirred at room temperature for 29 hours, concentrated in vacuo, diluted with ethyl acetate, washed sequentially with 0.1N sodium hydroxide solution and brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give a residue. Chromatography of the residue using silica gel and 20% to 25% ethyl acetate in hexanes solutions gives the title product as a white solid (0.86 g, mp 205°-208° C.).

후처리

  1. concentrationconcentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. washwashed sequentially with 0.1N sodium hydroxide solution and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto give a residue

출처 및 근거

ORD 기록
ord-dab398a0f9f7430081f72a7e6c45e221
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05438035

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