Hydrochloric Acid → N'-{4-[2-Chloro-4-(trifluoromethyl)phenoxy]phenyl}-N,N-dimethylurea

HRID 1679239

反応式

HRID 1679239 の反応式
[CH3:1][N:2]([CH3:6])[C:3](Cl)=[O:4].[Cl:7][C:8]1[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[CH:18][C:9]=1[O:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1.O.Cl>N1C=CC=CC=1>[CH3:1][N:2]([CH3:6])[C:3]([NH:15][C:14]1[CH:13]=[CH:12][C:11]([O:10][C:9]2[CH:18]=[CH:19][C:20]([C:22]([F:23])([F:24])[F:25])=[CH:21][C:8]=2[Cl:7])=[CH:17][CH:16]=1)=[O:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 6598Dimethylcarbamoyl ChlorideHCID 104693274-[2-Chloro-4-(trifluoromethyl)phenoxy]aniline

生成物 1

HCID 20362098N'-{4-[2-Chloro-4-(trifluoromethyl)phenoxy]phenyl}-N,N-dimethylurea収率 89%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

13 g (0.14 mole) of dimethylcarbamic acid chloride were added dropwise to 29 g (0.1 mole) of 4-(2-chloro-4-trifluoromethyl-phenoxy)-aniline, dissolved in 50 ml of pyridine, at 0° C. The mixture was warmed to 70°-75° C for half an hour, the bulk of the pyridine was stripped off in vacuo and the residue was poured into water and acidified with dilute hydrochloric acid. The precipitate was filtered off, dried and recrystallized from toluene. 29 g (89% of theory) of N,N-dimethyl-N'-[4-(2-chloro-4-trifluoromethylphenoxy)-phenyl]-urea were obtained as pink crystals of melting point 140° C.

後処理

  1. temperatureThe mixture was warmed to 70°-75° C for half an hour
  2. filtrationThe precipitate was filtered off
  3. customdried
  4. customrecrystallized from toluene

出典と根拠

ORDレコード
ord-5c3a23b6e3d148508c71b1315686de45
出典データセット
uspto-grants-1978_03
特許番号
US04080193

関連ノート

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