Benzyl chloroformate → Carbamic acid, (6-hydroxyhexyl)-, phenylmethyl ester

HRID 442625

반응식

HRID 442625 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][OH:8].C(=O)([O-])[O-].[K+].[K+].[CH2:15]([O:22][C:23](Cl)=[O:24])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>O.ClCCl>[C:23]([NH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][OH:8])([O:22][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:24]

참가 물질

6

반응물 3

HCID 10387Benzyl chloroformateHCID 11430Potassium CarbonateHCID 199606-Amino-1-hexanol

생성물 1

HCID 4184071Carbamic acid, (6-hydroxyhexyl)-, phenylmethyl ester

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

6-Aminohexan-1-ol (11.7 g, 100 mmol) and potassium carbonate (16.58 g, 120 mmol) were dissolved in 100 mL water and 70 mL dichloromethane. Benzylchloroformate (14.27 mL, 100 mmol) was added dropwise over 30 minutes at a temperature of 25°-30° C. The resulting mixture stood overnight, then the dichloromethane layer was separated, washed with water (3×200 mL), 2N HCl (3×50 mL) and finally with water (3×100 mL), dried, and evaporated to give a white solid. The solid was recrystallized in hexane-ethylacetate (8:2) to give a solid, which was collected and dried under vacuum at room temperature. Yield: 23 g (91%).

후처리

  1. customthe dichloromethane layer was separated
  2. washwashed with water (3×200 mL), 2N HCl (3×50 mL) and finally with water (3×100 mL)
  3. customdried
  4. customevaporated
  5. customto give a white solid
  6. customThe solid was recrystallized in hexane-ethylacetate (8:2)
  7. customto give a solid, which
  8. customwas collected
  9. customdried under vacuum at room temperature

출처 및 근거

ORD 기록
ord-8d199f257e1348d3a34d4ebea270c7bd
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05891862

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