Methanesulfonamide → 5-Bromo-N-methanesulfonylpentanamide

HRID 561772

반응식

HRID 561772 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

반응물 2

HCID 72879MethanesulfonamideHCID 5211735-Bromovaleryl chloride

생성물 1

HCID 202961415-Bromo-N-methanesulfonylpentanamide수율 88.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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

  1. temperaturewas cooled to room temperature
  2. washThe solution was washed with water, brine
  3. dry with materialdried over sodium sulfate
  4. filtrationThe solution was filtered
  5. customevaporated to 40 mL of solvent
  6. temperaturecooled to −15° C
  7. customA white precipitate formed
  8. 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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