Thionyl Chloride → (3aR,7S,7aR)-2-tert-butyloxycarbonyl-7-chloro-4,4-diphenylperhydroisoindole
反応式
[C:1]([O:5][C:6]([N:8]1[CH2:16][C@H:15]2[C@H:10]([C:11]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:12][CH2:13][C@@H:14]2O)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].S(Cl)([Cl:32])=O>>[C:1]([O:5][C:6]([N:8]1[CH2:9][C@@H:10]2[C@@H:15]([C@@H:14]([Cl:32])[CH2:13][CH2:12][C:11]2([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:16]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]参加物
3
実験手順
A solution of 1 g of (3aR,4S,7aR)-2-tert-butyloxycarbonyl-7,7-diphenyl-4-perhydroisoindolol in 10 cm3 of thionyl chloride is stirred for 3 hours at 80° C. The reaction mixture is then concentrated to dryness under reduced pressure (2.7 kPa). 1.03 g of (3aR,7S,7aR)-2-tert-butyloxycarbonyl-7-chloro-4,4-diphenylperhydroisoindole are obtained in the form of a solid which is used in the crude state in the next test.
後処理
- concentrationThe reaction mixture is then concentrated to dryness under reduced pressure (2.7 kPa)