3,4-Dichloroaniline → N-(3,4-Dichlorophenyl)prop-2-enamide

HRID 1384465

反応式

HRID 1384465 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[Cl:9])[NH2:5].C(N(CC)CC)C.[C:17](Cl)(=[O:20])[CH:18]=[CH2:19]>C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([NH:5][C:17](=[O:20])[CH:18]=[CH2:19])[CH:6]=[CH:7][C:8]=1[Cl:9]

参加物

5

反応物 3

HCID 72573,4-DichloroanilineHCID 8471TriethylamineHCID 13140Acryloyl chloride

生成物 1

HCID 13411358N-(3,4-Dichlorophenyl)prop-2-enamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A mixture of 3,4-dichloroaniline (3.6 g, 22.3 mmol) and 4.2 mL (30.2 mmol) of triethylamine in 20 mL of anhydrous methylene chloride was cooled to 0° C. under a nitrogen atmosphere and treated with acryloyl chloride (2.1 g, 23.2 mmol). The ice bath was removed and the mixture was stirred at room temperature for 1 hour after which time it was diluted with 120 mL of methylene chloride and washed with water and saturated aqueous sodium chloride (NaCl). After drying with calcium sulfate (CaSO4), the solvent was removed in vacuo to give a yellow solid, 4.84 g.

後処理

  1. customThe ice bath was removed
  2. additionwas diluted with 120 mL of methylene chloride
  3. washwashed with water and saturated aqueous sodium chloride (NaCl)
  4. dry with materialAfter drying with calcium sulfate (CaSO4)
  5. customthe solvent was removed in vacuo
  6. customto give a yellow solid, 4.84 g

出典と根拠

ORDレコード
ord-90163b68f8e64eb88eae794c08d34b46
出典データセット
uspto-grants-2001_07
特許番号
US06258953B1

関連ノート

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