Acetic Anhydride → 6,8-di-t-butyl-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester
反応式
[C:1]([C:5]1[CH:6]=[C:7]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:8]2[O:13][CH:12]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:11][C:10](=[O:19])[C:9]=2[CH:20]=1)([CH3:4])([CH3:3])[CH3:2].Cl(OC(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)(=O)(=O)=O.C(OC(=O)C)(=O)C.C(=O)(O)[O-].[Na+]>>[C:1]([C:5]1[CH:6]=[C:7]([C:21]([CH3:22])([CH3:24])[CH3:23])[C:8]2[O:13][C:12]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:11][C:10](=[O:19])[C:9]=2[CH:20]=1)([CH3:4])([CH3:3])[CH3:2]参加物
反応条件
- 温度
- 100 °C
実験手順
A mixture of 3.32 parts of 6,8-di-t-butyl-2,3-dihydro-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester, 1.56 parts of triphenylmethyl perchlorate and 30 parts of acetic anhydride was heated at 100° C for 30 minutes. After cooling, the reaction mixture was poured into sodium bicarbonate solution and the resulting mixture was washed with water, dried and the ether was evaporated to give an oil which was chromatographed on silica gel using a 1:1 mixture of chloroform and light petroleum (b.p. 40°-60° C) for elution. This yielded 0.14 parts of 6,8-di-t-butyl-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester, m.p. 130°-131.5° C (after crystallisation from light petroleum (b.p. 40°-60° C). This product was shown by spectral means to be the same as that prepared in Example 13.
後処理
- temperatureAfter cooling
- washthe resulting mixture was washed with water
- customdried
- customthe ether was evaporated
- customto give an oil which
- customwas chromatographed on silica gel using
- additiona 1:1 mixture of chloroform and light petroleum (b.p. 40°-60° C)
- washfor elution
出典と根拠
- ORDレコード
- ord-33a39b919ffc48f0ac3ccfb647023bd4
- 出典データセット
- uspto-grants-1977_10
- 特許番号
- US04055654
反応ノート
読み込み中…