Water → 5-Chloro-2-methyl-3-nitroaniline
반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]([CH3:11])=[C:6]([N+:8]([O-])=O)[CH:7]=1.O.S(S([O-])=O)([O-])=O.[Na+].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([N+:12]([O-:14])=[O:13])[C:5]([CH3:11])=[C:6]([NH2:8])[CH:7]=1참가 물질
5
실험 절차
5-Chloro-2-methyl-1,3-dinitro-benzene (1.96 g, from above) was suspended in methanol (80 mL) and water (20 mL) under N2. Sodium dithionite (5.51 g) was added portionwise and the mixture was stirred at room temperature for 3 hr. The reaction mixture was filtered and washed with methanol. The filtrate was then removed under reduced pressure and the residue was partitioned between ethyl acetate (150 mL) and brine (150 mL). The organic layer was dried over magnesium sulfate and evaporated to afford 5-chloro-2-methyl-3-nitro-phenylamine (1.45 g).
후처리
- filtrationThe reaction mixture was filtered
- washwashed with methanol
- customThe filtrate was then removed under reduced pressure
- customthe residue was partitioned between ethyl acetate (150 mL) and brine (150 mL)
- dry with materialThe organic layer was dried over magnesium sulfate
- customevaporated
출처 및 근거
- ORD 기록
- ord-0e51da76bfe7483a8f559cf29374efbe
- 출처 데이터셋
- uspto-grants-1999_09
- 특허 번호
- US05952362
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