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Triethylamine → HCID 58097356, 화합물

HRID 2067827
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HRID 2067827 반응식
[Br:1][C:2]1[CH:8]=[C:7]([O:9][C:10]([F:13])([F:12])[F:11])[C:5]([NH2:6])=[C:4]([Cl:14])[CH:3]=1.C(N(CC)CC)C.[C:22]([CH2:26][C:27](Cl)=[O:28])([CH3:25])([CH3:24])[CH3:23]>ClCCl>[Br:1][C:2]1[CH:8]=[C:7]([O:9][C:10]([F:12])([F:11])[F:13])[C:5]([NH:6][C:27](=[O:28])[CH2:26][C:22]([CH3:25])([CH3:24])[CH3:23])=[C:4]([Cl:14])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 815143,3-Dimethylbutanoyl chlorideHCID 177500654-Bromo-2-chloro-6-(trifluoromethoxy)aniline

생성물 1

HCID 58097356HCID 58097356, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 4-bromo-2-chloro-6-trifluoromethoxy-aniline (2.9 g, 10 mmol) and triethylamine (1.5 g, 15 mmol) in anhydrous dichloromethane (50 mL) was added dropwise tert-butylacetyl chloride (1.6 g, 12 mmol) with stirring at room temperature. The reaction mixture was stirred for 3 hours at room temperature, than the reaction mixture was diluted with dichloromethane and washed with water and dried over anhydrous sodium sulfate and evaporated to dryness under reduced pressure. The residue was purified by silica gel column (ISCO, hexane/EtOAc, 0-40%, 40 min) to give a white solid (3.6 g, 93%).

후처리

  1. stirringThe reaction mixture was stirred for 3 hours at room temperature, than the reaction mixture
  2. washwashed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated to dryness under reduced pressure
  5. customThe residue was purified by silica gel column (ISCO, hexane/EtOAc, 0-40%, 40 min)

출처 및 근거

ORD 기록
ord-aab51d2c09ce4305ae20db474c40ebe8
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08293911B2

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