Acetonitrile → 4-Bromo-1-methanesulfonyl-2-nitro-benzene

HRID 1988906노트

반응식

HRID 1988906 반응식
O[O:2][S:3]([O-:5])=O.[K+].CSC[C:10]1[CH:15]=[CH:14][C:13]([Br:16])=[CH:12][C:11]=1[N+:17]([O-:19])=[O:18].[C:20](#N)C>O>[Br:16][C:13]1[CH:14]=[CH:15][C:10]([S:3]([CH3:20])(=[O:5])=[O:2])=[C:11]([N+:17]([O-:19])=[O:18])[CH:12]=1

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 23707502Potassium hydroxy sulfiteHCID 686778004-Bromo-1-[(methylsulfanyl)methyl]-2-nitrobenzene2회

생성물 1

HCID 184343594-Bromo-1-methanesulfonyl-2-nitro-benzene

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A suspension of oxone (7.94 g) in water (16 ml) was added to a solution of (4-bromo-2-nitrophenyl)methyl methyl sulfide (Intermediate 72) (0.52 g) in acetonitrile (20 ml). The mixture was stirred for 5 h filtered and the residue was washed with ethyl acetate. The biphasic filtrate was separated, the aqueous layer was re-extracted with ethyl acetate (2×50 ml) and the combined organic extracts were washed with aqueous sodium metabisulphite (5%, 100 ml) water and brine. The solution was dried using a hydrophobic filter tube then concentrated under vacuum to give the title compound (0.35 g).

후처리

  1. filtrationfiltered
  2. washthe residue was washed with ethyl acetate
  3. customThe biphasic filtrate was separated
  4. extractionthe aqueous layer was re-extracted with ethyl acetate (2×50 ml)
  5. washthe combined organic extracts were washed with aqueous sodium metabisulphite (5%, 100 ml) water and brine
  6. customThe solution was dried
  7. concentrationthen concentrated under vacuum

출처 및 근거

ORD 기록
ord-45f7c83c91e7425d8ca56142dd2c53b3
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07642276B2

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