Bis(4-hydroxyphenyl)methane → HCID 20510578、化合物
反応式
[CH2:1]([N:5]1[C:9](=[O:10])[C:8]2([CH2:15][C:14]([CH3:17])([CH3:16])[N:13]([CH2:18][CH:19]3[O:21][CH2:20]3)[C:12]([CH3:23])([CH3:22])[CH2:11]2)[NH:7][C:6]1=[O:24])[CH2:2][CH2:3][CH3:4].[OH:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32][C:33]2[CH:38]=[CH:37][C:36]([OH:39])=[CH:35][CH:34]=2)=[CH:28][CH:27]=1.[H-].[Na+]>C(O)CC(C)C>[CH2:1]([N:5]1[C:9](=[O:10])[C:8]2([CH2:11][C:12]([CH3:22])([CH3:23])[N:13]([CH2:18][CH:19]([OH:21])[CH2:20][O:25][C:26]3[CH:27]=[CH:28][C:29]([CH2:32][C:33]4[CH:38]=[CH:37][C:36]([O:39][CH2:20][CH:19]([OH:21])[CH2:18][N:13]5[C:14]([CH3:17])([CH3:16])[CH2:15][C:8]6([NH:7][C:6](=[O:24])[N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[C:9]6=[O:10])[CH2:11][C:12]5([CH3:22])[CH3:23])=[CH:35][CH:34]=4)=[CH:30][CH:31]=3)[C:14]([CH3:17])([CH3:16])[CH2:15]2)[NH:7][C:6]1=[O:24])[CH2:2][CH2:3][CH3:4]参加物
5
実験手順
A mixture of 4.0 g of 3-butyl-8-(2,3-epoxypropyl)-7,7,9,9-tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione and 1.0 g of bis(p-hydroxyphenyl)methane in 5 ml of isopentyl alcohol with a catalytic amount of sodium hydride was refluxed for 10 hours. After completion of the reaction, the residue obtained by evaporating the solvent under reduced pressure from the reaction mixture was purified by column chromatography through silica gel eluted with a 1:1 by volume mixture of benzene and ethyl acetate, giving the desired Compound No. 351 in the form of white crystals melting at 202°-204° C.
後処理
- temperaturewas refluxed for 10 hours
- customAfter completion of the reaction
- customthe residue obtained
- customby evaporating the solvent under reduced pressure from the reaction mixture
- customwas purified by column chromatography through silica gel
- washeluted with a 1:1 by volume mixture of benzene and ethyl acetate
出典と根拠
- ORDレコード
- ord-ede89440b52340ad8bbc0763d430f07c
- 出典データセット
- uspto-grants-1983_02
- 特許番号
- US04371644
反応ノート
読み込み中…