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

HRID 1713497
ノート
印刷プレビュー

反応式

HRID 1713497 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6420Trichloroacetyl chlorideHCID 8471TriethylamineHCID 100093-Aminopyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7108aa33f66d415fb6c6ff0ecef25837
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795267B2

反応ノート

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