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[CH3:1][C:2]1[C:3]([OH:13])=[CH:4][CH:5]=[C:6]2[C:11]=1[O:10][C:9](=[O:12])[CH:8]=[CH:7]2.[CH3:14][C:15](O)([C:17]#[CH:18])[CH3:16].C1(C)C(C)=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>>[CH3:14][C:15]1([CH3:16])[O:13][C:3]2=[C:2]([CH3:1])[C:11]3[O:10][C:9](=[O:12])[CH:8]=[CH:7][C:6]=3[CH:5]=[C:4]2[CH:18]=[CH:17]1참가 물질
5
실험 절차
A solution prepared from 5.0 mmol of 8-methyl-7-hydroxycoumarin and 6.0 mmol of 2-methyl-3-butyn-2-ol in 40 ml of xylene containing 0.095 g (0.50 mmol) of p-toluenesulfonic acid was refluxed with magnetic stirring for 4 hours. The solvent was distilled off in vacuo and the oily contents of the flask chilled in an ice-salt water bath to induce crystallization. The white microneedles, 33% yield, were recrystallized from methanol to analytical purity, m.p. 105°-107° C. (lit. m.p. 106°-107° C.). The 1H-NMR spectrum was also identical to that reported, see P. Rodighiero et al., reference cited above.
후처리
- temperaturewas refluxed
- distillationThe solvent was distilled off in vacuo
- temperaturethe oily contents of the flask chilled in an ice-salt water bath
- customcrystallization
- customThe white microneedles, 33% yield, were recrystallized from methanol to analytical purity, m.p. 105°-107° C. (lit. m.p. 106°-107° C.)
출처 및 근거
- ORD 기록
- ord-cfc078f11e9c459db970a3fad57e8112
- 출처 데이터셋
- uspto-grants-1993_06
- 특허 번호
- US05216176
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