Cyanide → 1-n-Butyl-3-(m-chloro-alpha,alpha-dimethylbenzyl)-1-methylurea

HRID 614014ノート

反応式

HRID 614014 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][CH:13]=1)[C:5]([N:8]=[C:9]=[O:10])([CH3:7])[CH3:6].[C-]#N.[CH2:16]([NH:20][CH3:21])[CH2:17][CH2:18][CH3:19]>C1C=CC=CC=1>[CH2:16]([N:20]([CH3:21])[C:9]([NH:8][C:5]([CH3:7])([CH3:6])[C:4]1[CH:11]=[CH:12][CH:13]=[C:2]([Cl:1])[CH:3]=1)=[O:10])[CH2:17][CH2:18][CH3:19]

参加物

5

反応物 3

HCID 5975CyanideHCID 8068N-MethylbutylamineHCID 213298491-Chloro-3-(2-isocyanatopropan-2-yl)benzene

生成物 1

HCID 213298561-n-Butyl-3-(m-chloro-alpha,alpha-dimethylbenzyl)-1-methylurea収率 88.7%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

3.9 g of m-chloro-α,α-dimethylbenzyl isocyanate prepared from the corresponding cyanide in the same way as in Synthesis Example 1, was added to a solution of 1.8 g of N-n-butyl-N-methylamine in 20 ml of benzene and the mixture vigorously stirred. After allowing the mixture to stand overnight, the reaction solution was washed with a 2N aqueous hydrochloric acid solution, a 2N aqueous sodium hydroxide solution and water in that order, and the organic layer was dried over sodium sulfate. The layer was concentrated by evaporating off the solvent to obtain crystals, which were recrystallized from n-hexane to obtain 5.0 g of the title compound as crystals.

後処理

  1. washthe reaction solution was washed with a 2N aqueous hydrochloric acid solution
  2. dry with materiala 2N aqueous sodium hydroxide solution and water in that order, and the organic layer was dried over sodium sulfate
  3. concentrationThe layer was concentrated
  4. customby evaporating off the solvent
  5. customto obtain crystals, which
  6. customwere recrystallized from n-hexane

出典と根拠

ORDレコード
ord-c86957552dfc4e22b0cf4fa29a18d098
出典データセット
uspto-grants-1979_03
特許番号
US04143061

反応ノート

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