Ethanol → 4-Bromo-2,6-dichloro-3-methylaniline
反応式
[Cl:1][C:2]1[C:7]([CH3:8])=[C:6]([Br:9])[CH:5]=[C:4]([Cl:10])[C:3]=1[NH:11]C(=O)C.C(O)C.[OH-].[Na+]>O>[Cl:1][C:2]1[C:7]([CH3:8])=[C:6]([Br:9])[CH:5]=[C:4]([Cl:10])[C:3]=1[NH2:11]参加物
5
実験手順
A solution consisting of 2.07 g of N-(2,6-dichloro-4-bromo-3-methylphenyl)acetamide, 50 mL of ethanol, 25 mL of water and 25 mL of 50 percent NaOH were refluxed until hydrolysis was complete. The reaction mixture was cooled and extracted with ethyl ether. The extract was washed with water, dried over MgS04 and filtered. Removal of the solvent under reduced pressure gave 1.6 g of white solid. The product was purified by elution with pentane from a silica gel column and recrystallization from heptane (m.p. 67-69° C). 1H NMR (CCl4) δ7.33 (s, 1H), 4.40 (s, 2H, NH2), 2 40 (s, 3H, CH3).
後処理
- temperaturewere refluxed until hydrolysis
- temperatureThe reaction mixture was cooled
- extractionextracted with ethyl ether
- washThe extract was washed with water
- customdried over MgS04
- filtrationfiltered
- customRemoval of the solvent under reduced pressure
出典と根拠
- ORDレコード
- ord-62a3108f7e4c4b5684a28037ab1e4285
- 出典データセット
- uspto-grants-1991_11
- 特許番号
- US05068392
反応ノート
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