반응식
[CH3:1][N:2]1[CH:6]2[CH2:7][CH:8]([OH:10])[CH2:9][CH:3]1[CH2:4][CH2:5]2.C(N(C(C)C)CC)(C)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22].C(=O)([O-])[O-].[K+].[K+]>ClCCl.O.CCCCCCC>[CH3:1][N:2]1[CH:6]2[CH2:7][CH:8]([O:10][S:21]([CH3:20])(=[O:23])=[O:22])[CH2:9][CH:3]1[CH2:4][CH2:5]2참가 물질
반응물 4
생성물 1
시약·촉매·용매 3
반응 조건
- 온도
- 20 °C
실험 절차
Tropine (50 g) and diisopropylethylamine (48.05 g) in dichloromethane (0.5 L) were cooled to −10° C. Methane sulphonyl chloride (44.7 g) in dichloromethane (0.125 L) was added over 0.75 h at <−5° C. After 0.5 h a solution of potassium carbonate (75 g) in water (0.2 L) was added and the mixture warmed to 20° C. The phases were separated and the dichloromethane solution concentrated by distillation under reduced pressure at <20° C. to leave a residue whereby the dichloromethane content was 51% w/w. Heptane (0.05 L) was added and the solution cooled to 0° C. to crystallize the title compound. Further heptane (0.45 L) was added and the mixture kept under vacuum (350 mbar) at 20-25° C. until the dichloromethane content was 8% w/w. The mixture was cooled to 0° C. and stirred for 1 h. The product was isolated by filtration, washed and dried at <30° C. to give the title compound (68.5 g, 88.1%).
후처리
- customThe phases were separated
- concentrationthe dichloromethane solution concentrated by distillation under reduced pressure at <20° C.
- customto leave a residue whereby the dichloromethane content
- temperaturethe solution cooled to 0° C.
- customto crystallize the title compound
- additionFurther heptane (0.45 L) was added
- customkept under vacuum (350 mbar) at 20-25° C. until the dichloromethane content
- temperatureThe mixture was cooled to 0° C.
- customThe product was isolated by filtration
- washwashed
- customdried at <30° C.
출처 및 근거
- ORD 기록
- ord-79acaea70afd430ca372e42da7e5e71a
- 출처 데이터셋
- uspto-grants-2012_06
- 특허 번호
- US08207191B2
연결된 노트
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