Tetrahydrofuran → 3-Fluoro-2-methyl-6-nitroaniline
反応式
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]参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-fd03afd31c0541f1b48f5bd777a05cd4
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07709483B2
反応ノート
読み込み中…