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Trichloroacetyl chloride → 2,2,2-Trichloro-N-(pyridin-3-YL)acetamide

HRID 1713497
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HRID 1713497 반응식
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.C(N(CC)CC)C.[Cl:15][C:16]([Cl:21])([Cl:20])[C:17](Cl)=[O:18]>O1CCCC1>[Cl:15][C:16]([Cl:21])([Cl:20])[C:17]([NH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1)=[O:18]
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참가 물질

5

반응물 3

HCID 6420Trichloroacetyl chlorideHCID 8471TriethylamineHCID 100093-Aminopyridine

생성물 1

HCID 34477032,2,2-Trichloro-N-(pyridin-3-YL)acetamide수율 89%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a solution of 3-aminopyridine (1.0 g, 11 mmol) and triethylamine (1.3 g, 13 mmol) in tetrahydrofuran (30 mL) was added at 0° C. trichloroacetyl chloride (1.4 mL, 13 mmol), and the mixture was stirred at 0° C. for 20 minutes. The reaction solution was concentrated, and ethyl acetate was added to the residue. The resulting mixture was washed with water and saturated brine and dried over magnesium sulfate. The solid was filtered off, and the filtrate was concentrated. The residue was washed with diisopropyl ether and collected by filtration to obtain the title compound (2.3 g, yield 89%) as colorless powder.

후처리

  1. concentrationThe reaction solution was concentrated
  2. additionethyl acetate was added to the residue
  3. washThe resulting mixture was washed with water and saturated brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationThe solid was filtered off
  6. concentrationthe filtrate was concentrated
  7. washThe residue was washed with diisopropyl ether
  8. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-7108aa33f66d415fb6c6ff0ecef25837
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07795267B2

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