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

HRID 614014노트

반응식

HRID 614014 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c86957552dfc4e22b0cf4fa29a18d098
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04143061

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