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

HRID 596727ノート

反応式

HRID 596727 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-dac99c30401741b39d3cbf736e4bcb2c
出典データセット
uspto-grants-1977_03
特許番号
US04012225

反応ノート

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