4-Nitroaniline → 2-(2-chloroethoxy)-N-(4-nitrophenyl)acetamide

HRID 2246805노트

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HRID 2246805 반응식
Cl[C:2]1([Cl:8])[CH2:7][O:6][CH2:5][CH2:4][O:3]1.[N+:9]([C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1)([O-:11])=[O:10]>>[Cl:8][CH2:2][CH2:7][O:6][CH2:5][C:4]([NH:16][C:15]1[CH:17]=[CH:18][C:12]([N+:9]([O-:11])=[O:10])=[CH:13][CH:14]=1)=[O:3]

참가 물질

3

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온도
80 °C

실험 절차

1.53 g of a mixture of 2-chlorodioxene and 2,2-dichlorodioxane (molar ratio 1:1) are added to 1.00 g (7.24 mmol) of 4-nitroaniline, and the mixture is heated to 80° C. with stirring. A solid brown mass forms within one hour and becomes liquid again and crystallises within the following 12 hours. The crude product is recrystallised from ethanol with addition of water, giving 1.80 g of 2-(2-chloroethoxy)-N-(4-nitrophenyl)acetamide (“A1”) as yellowish crystals, m.p. 101-102° C. 1H-NMR (d6-DMSO): δ=3.82 (m; 4H), 4.23 (s; 2H), 7.91 (d, J=9 Hz, 2H), 8.23 (d, J=9 Hz, 2H), 10.34 (s, 1H).

후처리

  1. customcrystallises within the following 12 hours
  2. customThe crude product is recrystallised from ethanol with addition of water

출처 및 근거

ORD 기록
ord-f977f05c02f14736b1bdb0c0309a60a6
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07687624B2

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