반응식
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[CH3:12][O:13][C:14]1[CH:23]=[C:22]2[C:17]([CH2:18][CH2:19][CH:20]([CH2:24][OH:25])[CH2:21]2)=[CH:16][CH:15]=1>N1C=CC=CC=1>[CH3:12][O:13][C:14]1[CH:23]=[C:22]2[C:17]([CH2:18][CH2:19][CH:20]([CH2:24][O:25][S:7]([C:4]3[CH:5]=[CH:6][C:1]([CH3:11])=[CH:2][CH:3]=3)(=[O:9])=[O:8])[CH2:21]2)=[CH:16][CH:15]=1참가 물질
실험 절차
20.96 g (110 mmol) of p-toluenesulphonic acid chloride are added at room temperature, while stirring, to a solution of 19.2 g (100 mmol) of 7-methoxy-1,2,3,4-tetrahydro-naphthalene-2-methanol in 80 ml of absolute pyridine, the slightly exothermic reaction being maintained at room temperature with an ice bath. The reaction mixture is stirred at room temperature for 1 hour to complete the reaction and is then diluted with ice-water and extracted with diethyl ether. The organic phase is washed while ice-cold with 2N hydrochloric acid and water, is dried over sodium sulphate, filtered and concentrated by evaporation under reduced pressure. The resulting oil is crystallised from diethyl ether/pentane to yield p-toluenesulphonic acid (7-methoxy-1,2,3,4-tetrahydro-naphth-2-ylmethyl) ester of m.p. 64°-66 °.
후처리
- customthe slightly exothermic reaction
- customthe reaction
- extractionextracted with diethyl ether
- washThe organic phase is washed while ice-cold with 2N hydrochloric acid and water
- dry with materialis dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated by evaporation under reduced pressure
- customThe resulting oil is crystallised from diethyl ether/pentane
출처 및 근거
- ORD 기록
- ord-be662b22142e48788f1767714c267279
- 출처 데이터셋
- uspto-grants-1989_05
- 특허 번호
- US04833169
연결된 노트
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