Chloral → N'-(2-Fluorophenyl)-N-methyl-N-(1,2,2,2-tetrachloroethyl)urea

HRID 596727노트

반응식

HRID 596727 반응식
[CH3:1][NH:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:4].O=[CH:14][C:15]([Cl:18])([Cl:17])[Cl:16].S(Cl)([Cl:21])=O>C(OCC)C>[CH3:1][N:2]([CH:14]([Cl:21])[C:15]([Cl:18])([Cl:17])[Cl:16])[C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:4]

참가 물질

5

반응물 3

HCID 6407ChloralHCID 24386Thionyl ChlorideHCID 676515N-(2-fluorophenyl)-N'-methylurea

생성물 1

HCID 12906107N'-(2-Fluorophenyl)-N-methyl-N-(1,2,2,2-tetrachloroethyl)urea

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

N-methyl-N'-o-fluorophenyl urea (16.8 g, 0.1 mol) was combined with 22.5 g (0.15 mol) chloral and 18.0 g (0.15 mol) thionyl chloride. After several minutes an exothermicity was noted and the reaction mixture became a homogenous yellow oil. After 5 minutes more, a precipitate began to form. After 11/2 hours a 3:1 mixture of diethyl ether:petroleum ether was added and the product was collected on a filter and dried. The product weighed 25 g, melted at 130°-141° C. and analyzed as follows: %Cl, calculated 35.7, found 37.3; %N, calculated 9.5, found 9.5. The product is the sixth compound tabulated in Table I.

후처리

  1. waitAfter several minutes an exothermicity was noted
  2. customto form
  3. customthe product was collected on
  4. filtrationa filter
  5. customdried

출처 및 근거

ORD 기록
ord-dac99c30401741b39d3cbf736e4bcb2c
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012225

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