Hydrochloric Acid → N,N'-Bis[4-(chloromethyl)phenyl]-N,N'-dimethylurea

HRID 570028ノート

反応式

HRID 570028 の反応式
[CH3:1][N:2]([C:15]1[CH:20]=[CH:19][C:18](CO)=[CH:17][CH:16]=1)[C:3]([N:5]([CH3:14])[C:6]1[CH:11]=[CH:10][C:9]([CH2:12]O)=[CH:8][CH:7]=1)=[O:4].[ClH:23].CCCCCC.[CH:30]([Cl:33])(Cl)Cl>>[CH3:1][N:2]([C:15]1[CH:20]=[CH:19][C:18]([CH2:30][Cl:33])=[CH:17][CH:16]=1)[C:3]([N:5]([CH3:14])[C:6]1[CH:11]=[CH:10][C:9]([CH2:12][Cl:23])=[CH:8][CH:7]=1)=[O:4]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 6212ChloroformHCID 8058HexaneHCID 54431102HCID 54431102、化合物

生成物 1

HCID 20064895N,N'-Bis[4-(chloromethyl)phenyl]-N,N'-dimethylurea

実験手順

A solution of 10 g N,N'-dimethyl-N,N'-bis(p-hydroxymethylphenyl) urea in 250 ml CHCl3 was stirred vigorously for two hours with 250 ml conc. HCl. The layers were separated, and the organic phase was washed with dilute HCl, dried, and stripped to give a yellow oil. Trituration with hexane caused the product to crystallize. Filtration, washing with hexane, and air drying gave 3.5 g of a fluffy-white crystalline solid which was pure by TLC, m.p. 72°-73° C.

後処理

  1. customThe layers were separated
  2. washthe organic phase was washed with dilute HCl
  3. customdried
  4. customto give a yellow oil
  5. customto crystallize
  6. filtrationFiltration
  7. washwashing with hexane, and air
  8. customdrying

出典と根拠

ORDレコード
ord-30702cb4383c4c449f2d0143ecfd9834
出典データセット
uspto-grants-1988_03
特許番号
US04734458

反応ノート

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