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Triethylamine → HCID 86649635, 화합물

HRID 880699
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HRID 880699 반응식
[Br:1][C:2]1[CH:8]=[C:7]([O:9][C:10]([F:13])([F:12])[F:11])[C:5](N)=[C:4]([Cl:14])[CH:3]=1.C([N:17](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:13])([F:12])[F:11])[C:5]([CH:26]([C:22]([CH3:25])([CH3:24])[CH3:23])[C:27]([NH2:17])=[O:28])=[C:4]([Cl:14])[CH:3]=1
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참가 물질

5

반응물 3

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

생성물 1

HCID 86649635HCID 86649635, 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-433a9f37a1134e9887ceeb673a4c0f8f
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08993593B2

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