Dimethylformamide → N-(2-Chloroethyl)-2,6-dinitro-N-2-propen-1-yl-4-(trifluoromethyl)benzenamine

HRID 441785ノート

反応式

HRID 441785 の反応式
O[CH2:2][CH2:3][N:4]([CH2:21][CH:22]=[CH2:23])[C:5]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([C:14]([F:17])([F:16])[F:15])=[CH:7][C:6]=1[N+:18]([O-:20])=[O:19].CN(C)C=O.S(Cl)([Cl:31])=O>C1C=CC=CC=1>[Cl:31][CH2:2][CH2:3][N:4]([CH2:21][CH:22]=[CH2:23])[C:5]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([C:14]([F:17])([F:16])[F:15])=[CH:7][C:6]=1[N+:18]([O-:20])=[O:19]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 53750272HCID 53750272、化合物

生成物 1

HCID 53970178N-(2-Chloroethyl)-2,6-dinitro-N-2-propen-1-yl-4-(trifluoromethyl)benzenamine

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

16.7 parts by weight of N-hydroxyethyl-N-allyl-2,6-dinitro-4-trifluoromethylaniline is dissolved in 50 parts by weight of benzene. After adding 1 part by weight of dimethylformamide and dripping in 30 parts by weight of thionyl chloride at room temperature the whole is boiled for two hours under reflux. The volatile constituents are distilled off from the reaction mixture at 20 mm Hg, the residue is taken up in ethyl acetate, the solution is washed with ice-water, then with 10% sodium bicarbonate solution and finally again with water and the organic phase is dried over sodium sulfate.

後処理

  1. temperatureunder reflux
  2. distillationThe volatile constituents are distilled off from the reaction mixture at 20 mm Hg
  3. washthe solution is washed with ice-water
  4. dry with materialwith 10% sodium bicarbonate solution and finally again with water and the organic phase is dried over sodium sulfate

出典と根拠

ORDレコード
ord-7a6ede6311244f36bf73244151260b1e
出典データセット
uspto-grants-1977_08
特許番号
US04042628

反応ノート

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