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Triethylamine → Ethyl 2-chloro-3,4-dimethoxyphenethylcarbamate

HRID 525844
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반응식

HRID 525844 반응식
[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([O:10][CH3:11])[CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][NH2:14].C(N(CC)CC)C.Cl[C:23]([O:25][CH2:26][CH3:27])=[O:24]>ClCCl>[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([O:10][CH3:11])[CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][NH:14][C:23](=[O:24])[O:25][CH2:26][CH3:27]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 30177522-Chloro-3,4-dimethoxyphenethylamine

생성물 1

HCID 86732714Ethyl 2-chloro-3,4-dimethoxyphenethylcarbamate수율 97%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To the solution of 2-(2-chloro-3,4-dimethoxyphenyl)ethanamine (2.8 g, 12.98 mmol) in dichloromethane (DCM) (40 mL) at 0° C. was added triethylamine (1.990 mL, 14.28 mmol) and ethyl chloroformate (1.371 mL, 14.28 mmol). The reaction mixture was stirred at room temperature for 12 hours. The resulting mixture was washed with water, brine, dried over magnesium sulfate and chromatographed to give ethyl 2-chloro-3,4-dimethoxyphenethylcarbamate (1.7 g, 5.91 mmol, 97% yield). LCMS (M+H)+: 288.1

후처리

  1. washThe resulting mixture was washed with water, brine
  2. dry with materialdried over magnesium sulfate
  3. customchromatographed

출처 및 근거

ORD 기록
ord-6d8bc861aceb42b687017dea8e3f2a98
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09340556B2

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