Ethyl Acetate → Benzyl (3-hydroxycyclohexyl)carbamate

HRID 1013812노트

반응식

HRID 1013812 반응식
[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH:4]([NH2:8])[CH2:3]1.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C.Cl[C:22]([O:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:23]>O>[CH2:25]([O:24][C:22](=[O:23])[NH:8][CH:4]1[CH2:5][CH2:6][CH2:7][CH:2]([OH:1])[CH2:3]1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 10387Benzyl chloroformateHCID 11430Potassium CarbonateHCID 112404593-Aminocyclohexanol

생성물 1

HCID 14476840Benzyl (3-hydroxycyclohexyl)carbamate수율 88.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Treat a mixture of 3-hydroxycyclohexyl amine (10 g, 86.96 mmol), potassium carbonate (18 g, 130 mmol), ethyl acetate (150 mL) and water (70 mL) with benzyl chloroformate (22.17 g, 130 mmol). Stir the reaction at room temperature for 12 hours. Separate the organic layer, dry the organic over sodium sulfate, filter and concentrate. Add diethyl ether to the residuer. Filter the resulting white precipitate and air dry to afford 19.1 g of the title compound (88%). MS (m/z): 250 (M+).

후처리

  1. additionTreat
  2. customthe reaction at room temperature for 12 hours
  3. customSeparate the organic layer
  4. dry with materialdry the organic over sodium sulfate
  5. filtrationfilter
  6. concentrationconcentrate
  7. filtrationFilter the resulting white precipitate and air
  8. customdry

출처 및 근거

ORD 기록
ord-804318bcbfbb46449e650c709fde728c
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981918B2

반응 노트

불러오는 중…