Sodium hydride → 2-Bromo-N-Methylsulfonylacetamide

HRID 53668노트

반응식

HRID 53668 반응식
[H-].[Na+].[CH3:3][S:4]([NH2:7])(=[O:6])=[O:5].[Br:8][CH2:9][C:10](Br)=[O:11]>O1CCCC1>[Br:8][CH2:9][C:10]([NH:7][S:4]([CH3:3])(=[O:6])=[O:5])=[O:11]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 61147Bromoacetyl bromideHCID 72879Methanesulfonamide

생성물 1

HCID 2629442-Bromo-N-Methylsulfonylacetamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Sodium hydride (1.68 g×60% ) was added to a stirred solution of methanesulfonamide (2.0 g) in dry tetrahydrofuran (20 ml) at room temperature. The resulting solution was stirred at room temperature for 1 hour, as which time it was treated with a solution of bromoacetyl bromide (4.2 g) in dry tetrahydrofuran (10 ml). After 1 hour the solvent was removed under reduced pressure and the residue taken up in water and acidified to pH3. The acidic solution was extracted into ethyl acetate, dried (MgSO4), filtered and the solvent removed under reduced pressure. Recrystallisation from isopropanol afforded the product as white needles: mp 112°-114° C.

후처리

  1. customAfter 1 hour the solvent was removed under reduced pressure
  2. extractionThe acidic solution was extracted into ethyl acetate
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent removed under reduced pressure
  6. customRecrystallisation from isopropanol

출처 및 근거

ORD 기록
ord-575b933edd854cfcb80aab968d02232c
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620989

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