Methanesulfonamide → 5-Bromo-N-methanesulfonylpentanamide
반응식
[CH3:1][S:2]([NH2:5])(=[O:4])=[O:3].[Br:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11](Cl)=[O:12]>C(OCC)(=O)C>[Br:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([NH:5][S:2]([CH3:1])(=[O:4])=[O:3])=[O:12]참가 물질
4
반응 조건
- 온도
- 87.5 °C
실험 절차
A mixture consisting of methanesulfonamide (4.76 g) and 5-bromovaleric acid chloride (10 g) was heated at 85-90° C. for one hour, was cooled to room temperature, and was diluted with ethyl acetate (75 mL). The solution was washed with water, brine, and dried over sodium sulfate. The solution was filtered and evaporated to 40 mL of solvent, then cooled to −15° C. A white precipitate formed, which was collected by filtration to afford the title intermediate (11.4 g, 88%) as a white solid; melting point 98-100° C.
후처리
- temperaturewas cooled to room temperature
- washThe solution was washed with water, brine
- dry with materialdried over sodium sulfate
- filtrationThe solution was filtered
- customevaporated to 40 mL of solvent
- temperaturecooled to −15° C
- customA white precipitate formed
- filtrationwhich was collected by filtration
출처 및 근거
- ORD 기록
- ord-4ccd0fc749d9494d93f44d84999ebb6f
- 출처 데이터셋
- uspto-grants-2011_11
- 특허 번호
- US08063240B2
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