反応式
[C:1]([C:4]1[CH:5]=[C:6]([CH:11]=[CH:12][CH:13]=1)[NH:7][C:8](=[O:10])[CH3:9])(=[O:3])[CH3:2].[Br:14]Br>C(Cl)(Cl)Cl>[Br:14][CH2:2][C:1]([C:4]1[CH:5]=[C:6]([CH:11]=[CH:12][CH:13]=1)[NH:7][C:8](=[O:10])[CH3:9])=[O:3]参加物
4
実験手順
To a stirred solution of 110.0 g. (0.62 mole) of 3'-acetylacetanilide in 2400 ml. of chloroform is added dropwise a solution of 33.0 ml. (102.9 g; 0.644 mole) of bromine in 240 ml. of chloroform. The solution is stirred one hour and the resultant precipitate is then filtered, washed with ether and dried. The solid is stirred in a large volume of water to give an oily precipitate which crystallizes on further stirring. The solid is filtered, washed with water and then 2-propanol. The dried product weighs 148.34 g., and is recrystallized from 2-propanol to give the product, melting point 108.5°-110° C. Analysis: Calcd, for C10H10BrNO2 : Calcd: C, 46.90; H, 3.94; Br, 31.20; N, 5.47. Found: C, 47.12; H, 3.94; Br, 31.21; N, 5.47.
後処理
- filtrationthe resultant precipitate is then filtered
- washwashed with ether
- customdried
- stirringThe solid is stirred in a large volume of water
- customto give an oily precipitate which
- customcrystallizes on further stirring
- filtrationThe solid is filtered
- washwashed with water
- custom, and is recrystallized from 2-propanol
- customto give the product, melting point 108.5°-110° C
出典と根拠
- ORDレコード
- ord-de425ded540241f9953b6087d2c3a356
- 出典データセット
- uspto-grants-1977_03
- 特許番号
- US04014892
関連ノート
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