反応式
[CH2:1]([O:13][C:14]1[CH:22]=[CH:21][C:17]([C:18](O)=[O:19])=[CH:16][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].S(Cl)([Cl:25])=O>>[CH2:1]([O:13][C:14]1[CH:22]=[CH:21][C:17]([C:18]([Cl:25])=[O:19])=[CH:16][CH:15]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]参加物
実験手順
p-n-Dodecyloxybenzoic acid (8 g) together with thionyl chloride (20 ml) were heated under reflux for 2 hours, followed by distilling off excess thionyl chloride to obtain p-n-dodecyloxybenzoic acid chloride, which was made up into a toluene solution thereof without any particular purification. On the other hand, optically active hydroquinonemono(2-methylbutyl) ether (4.7 g) obtained above in the item (I) was dissolved in pyridine (30 ml). To this solution kept at 0° C. was dropwise added the toluene solution of p-n-dodecyloxybenzoic acid chloride obtained above, followed by heating the mixture at 90° C. for 2 hours for reaction, separating the resulting esterified substance in a conventional manner, and twice repeating recrystallization to obtain colorless crystals of p-n-dodecyloxybenzoic acid p'-(2-methylbutyloxy)phenyl ester (C-SC* point, 50.5° C.; SC*-SA point, 51.2° C.; SA-I point, 65° C.; and [α]D25° =+5.2° (as measured in chloroform solution)) (6.5 g). Further its elemental analysis values accorded well with its theoretical values as follows:
後処理
- temperatureunder reflux for 2 hours
- distillationby distilling off excess thionyl chloride
出典と根拠
- ORDレコード
- ord-506744beace94d5b9e4d01f88d14d550
- 出典データセット
- uspto-grants-1989_04
- 特許番号
- US04820444
関連ノート
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