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Carbon Dioxide → 4-[4-(Trifluoromethoxy)phenoxy]piperidine

HRID 1799509
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HRID 1799509 반응식
[OH-].[K+].C(OC([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:25])([F:24])[F:23])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)C.C(=O)=O>C(O)C(C)C>[F:25][C:22]([F:23])([F:24])[O:21][C:18]1[CH:19]=[CH:20][C:15]([O:14][CH:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)=[CH:16][CH:17]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 280Carbon DioxideHCID 14797Potassium HydroxideHCID 68485568HCID 68485568, 화합물

생성물 1

HCID 161154394-[4-(Trifluoromethoxy)phenoxy]piperidine

시약·촉매·용매 1

HCID 6560Isobutanol용매2회

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온도
100 °C

실험 절차

Potassium hydroxide (10.7 g) was heated to 100° C., and dissolved in isobutanol (15 mL). An isobutanol (25 mL) solution of 1-ethoxycarbonyl-4-(4-trifluoromethoxyphenoxy)piperidine (12.03 g) was dropwise added thereto while noticing generation of carbon dioxide gas. After the dropwise addition, the mixture was heated and stirred at 100° C. for 2 hours; then the solvent was concentrated; and toluene (40 mL) was added to the obtained residue. The toluene solution was washed with water (40 mL×2), and then the solvent was concentrated under reduced pressure to obtain a target compound as a light orange solid substance. The yield amount was 5.73 g (98% based on trifluoromethoxyphenol).

후처리

  1. additionAfter the dropwise addition
  2. temperaturethe mixture was heated
  3. concentrationthen the solvent was concentrated
  4. additionand toluene (40 mL) was added to the obtained residue
  5. washThe toluene solution was washed with water (40 mL×2)
  6. concentrationthe solvent was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-16448fe0c2ea43fa9677a436a9968a9c
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08344148B2

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