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

HRID 1763204ノート

反応式

HRID 1763204 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 1 1/2 hours, a 3:1 mixture of diethyl ether:petroleum ether was added and the product was collected of a filter and dried. The solid, which weighed 25 g, melted at 130°-141° C and analyzed as follows: %Cl, calc. 35.7, found 37.3; %N, calc. 9.5, found 9.5.

後処理

  1. waitAfter several minutes
  2. customto form
  3. customthe product was collected of
  4. filtrationa filter
  5. customdried

出典と根拠

ORDレコード
ord-2d492ce9844e484ba3977a01b60dce06
出典データセット
uspto-grants-1978_09
特許番号
US04111683

反応ノート

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