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

HRID 1384465

반응식

HRID 1384465 반응식
[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]

참가 물질

5

반응물 3

HCID 72573,4-DichloroanilineHCID 8471TriethylamineHCID 13140Acryloyl chloride

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-90163b68f8e64eb88eae794c08d34b46
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06258953B1

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