Tetrahydrofuran → 3-Fluoro-2-methyl-6-nitroaniline
반응식
ClCC([NH:5][C:6]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[C:8]([F:15])[C:7]=1[CH3:16])=O.[OH-].[Na+].O1CCCC1>O>[F:15][C:8]1[C:7]([CH3:16])=[C:6]([C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=1)[NH2:5]참가 물질
5
실험 절차
2-Chloro-N-(3-fluoro-2-methyl-6-nitrophenyl)acetamide (prepared from 47.2 g of 2-chloro-N-(3-fluoro-2-methylphenyl)acetamide, ca. 234 mmol) was suspended in water (220 ml) then treated with aqueous sodium hydroxide solution (12.5M, 110 ml, 1.37 mol). Tetrahydrofuran (110 ml) was added, then the mixture was heated to reflux for 5 hours, then evaporated (removing most of the tetrahydrofuran). The yellow solid was filtered off and washed with water until washing were non-alkaline. Drying in vacuo afforded a yellow solid (32.3 g, 81% over 2 steps) containing ˜13% isomer.
후처리
- temperaturethe mixture was heated
- temperatureto reflux for 5 hours
- customevaporated (
- customremoving most of the tetrahydrofuran)
- filtrationThe yellow solid was filtered off
- washwashed with water
- washuntil washing
- customDrying in vacuo
- customafforded a yellow solid (32.3 g, 81% over 2 steps)
- additioncontaining ˜13% isomer
출처 및 근거
- ORD 기록
- ord-fd03afd31c0541f1b48f5bd777a05cd4
- 출처 데이터셋
- uspto-grants-2010_05
- 특허 번호
- US07709483B2
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