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Acetyl chloride → tert-Butyl {2-(acetylamino)-1-[3-(trifluoromethyl)phenyl]ethyl}carbamate

HRID 2402773
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HRID 2402773 반응식
[NH2:1][CH2:2][CH:3]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:13])([F:12])[F:11])[CH:5]=1.C(N(CC)C(C)C)(C)C.[C:31](Cl)(=[O:33])[CH3:32]>ClCCl.C(OCC)(=O)C>[C:31]([NH:1][CH2:2][CH:3]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:18])([CH3:20])[CH3:19])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:13])([F:12])[F:11])[CH:5]=1)(=[O:33])[CH3:32]
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참가 물질

6

반응물 3

HCID 6367Acetyl chlorideHCID 81531DiisopropylethylamineHCID 43094068tert-butyl N-{2-amino-1-[3-(trifluoromethyl)phenyl]ethyl}carbamate

생성물 1

HCID 59536855tert-Butyl {2-(acetylamino)-1-[3-(trifluoromethyl)phenyl]ethyl}carbamate수율 100%

시약·촉매·용매 2

HCID 6344Dichloromethane용매
HCID 8857
Ethyl Acetate
용매

실험 절차

Of the compound from Example 22A, 75 mg (0.25 mmol) were introduced in 2.5 ml of dichloromethane together with 60 μl (0.35 mmol) of N,N-diisopropylethylamine and admixed at RT with 21 μl (0.30 mmol) of acetyl chloride. The mixture was stirred at RT for 1 h. The reaction mixture was diluted with ethyl acetate and washed in succession twice each with 1N hydrochloric acid, saturated aqueous sodium hydrogen carbonate solution, and then with saturated aqueous sodium chloride solution, dried over sodium sulphate and freed from the solvent on a rotary evaporator. Further drying in an HV gave 88 mg of the title compound (100% of theory).

후처리

  1. washwashed in succession twice each with 1N hydrochloric acid, saturated aqueous sodium hydrogen carbonate solution
  2. dry with materialwith saturated aqueous sodium chloride solution, dried over sodium sulphate
  3. customfreed from the solvent on a rotary evaporator
  4. customFurther drying in an HV

출처 및 근거

ORD 기록
ord-d937a53568b94a4ca06cfb3e4557fe9a
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08796324B2

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