2-Amino-4-chlorophenol → 2-Acetylamino-4-chlorophenol
反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[OH:9].[C:10]([O:14]C)(C)(C)[CH3:11]>>[Cl:8][C:6]1[CH:5]=[CH:4][C:3]([OH:9])=[C:2]([NH:1][C:10](=[O:14])[CH3:11])[CH:7]=1参加物
3
反応条件
- 温度
- 22.5 °C
実験手順
143.6 g (1 mole) of 2-amino-4-chlorphenol was suspended in 550 ml of methyl t-butyl ether under mild nitrogen purge. The mixture was heated to reflux until the material was dissolved. After 40 minutes, 112.3 g of acetic anhydride was added. After the addition the mixture was cooled to 20-25° C. in one hour. After stirring for an additional hour the mixture was cooled to 0-5° C. under stirring and kept on this temperature for an additional hour. The product was filtered off, washed with 200 ml of methyl t-butyl ether twice and dried at 50° C. and 100 mbar under a gentle nitrogen stream till dry. Yield about 92%.
後処理
- custompurge
- temperatureThe mixture was heated
- temperatureto reflux until the material
- dissolutionwas dissolved
- addition112.3 g of acetic anhydride was added
- additionAfter the addition the mixture
- temperaturewas cooled to 0-5° C.
- stirringunder stirring
- waitkept on this temperature for an additional hour
- filtrationThe product was filtered off
- washwashed with 200 ml of methyl t-butyl ether twice
- customdried at 50° C.
- customtill dry
出典と根拠
- ORDレコード
- ord-e1db0f8216b2401a958126e0e678b5bd
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07423040B2
反応ノート
読み込み中…