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1-Chloroethyl chloroformate → 4-(2-Chlorophenyl)-4-methylpiperidine

HRID 557010
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반응식

HRID 557010 반응식
C([N:8]1[CH2:13][CH2:12][C:11]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[Cl:21])([CH3:14])[CH2:10][CH2:9]1)C1C=CC=CC=1.ClC(OC(Cl)C)=O>ClCCCl>[Cl:21][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[C:11]1([CH3:14])[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1
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참가 물질

4

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 23136891HCID 23136891, 화합물

생성물 1

HCID 231369824-(2-Chlorophenyl)-4-methylpiperidine수율 73.4%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

A solution of 1-benzyl-4-(2-chloro-phenyl)-4-methyl-piperidine (0.59 g, 1.95 mmol) in 1,2-dichloroethane (10 mL) was treated with 1-chloroethyl chloroformate (0.28 mL, 2.6 mmol). This mixture was stirred for 12 hr at reflux, then evaporated in vacuo. The residue was redissolved in methanol (10 mL) and heated to reflux for 1 hr, then evaporated in vacuo. The resulting brown solid (the hydrochloride salt) was washed with ethyl acetate, then freebased with ethyl acetate/sodium hydroxide to yield 0.30 g (72%) of the title compound, ESI-MS m/z: 246 [M+1].

후처리

  1. temperatureat reflux
  2. customevaporated in vacuo
  3. dissolutionThe residue was redissolved in methanol (10 mL)
  4. temperatureheated
  5. temperatureto reflux for 1 hr
  6. customevaporated in vacuo
  7. washThe resulting brown solid (the hydrochloride salt) was washed with ethyl acetate

출처 및 근거

ORD 기록
ord-04955d163fcf4e76bb17117f9e7e472a
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08058287B2

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