Hydrochloric Acid → N,N'-Bis[4-(chloromethyl)phenyl]-N,N'-dimethylurea
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- customThe layers were separated
- washthe organic phase was washed with dilute HCl
- customdried
- customto give a yellow oil
- customto crystallize
- filtrationFiltration
- washwashing with hexane, and air
- customdrying
출처 및 근거
- ORD 기록
- ord-30702cb4383c4c449f2d0143ecfd9834
- 출처 데이터셋
- uspto-grants-1988_03
- 특허 번호
- US04734458
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