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

HRID 441785노트

반응식

HRID 441785 반응식
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]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 53750272HCID 53750272, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7a6ede6311244f36bf73244151260b1e
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04042628

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