Sodium Bromide → 6-bromomethyl-3,5-dimethyl-4-methoxymethoxy-2H-pyran-2-one

HRID 1357187노트

반응식

HRID 1357187 반응식
[Br-:1].[Na+].[CH3:3][C:4]1[C:5](=[O:21])[O:6][C:7]([CH2:15]OS(C)(=O)=O)=[C:8]([CH3:14])[C:9]=1[O:10][CH2:11][O:12][CH3:13]>CN(C=O)C>[Br:1][CH2:15][C:7]1[O:6][C:5](=[O:21])[C:4]([CH3:3])=[C:9]([O:10][CH2:11][O:12][CH3:13])[C:8]=1[CH3:14]

참가 물질

4

반응물 2

HCID 253881Sodium BromideHCID 120829703,5-dimethyl-4-methoxymethoxy-6-(methylsulfonyloxy)methyl-2H-pyran-2-one

생성물 1

HCID 120829716-bromomethyl-3,5-dimethyl-4-methoxymethoxy-2H-pyran-2-one

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Sodium bromide (500 mg) was added to a solution of 3,5-dimethyl-4-methoxymethoxy-6-(methylsulfonyloxy)methyl-2H-pyran-2-one (1.35 g) in DMF (20 ml), and after the stirring the mixture at room temperature for one hour, the reaction solution was concentrated under reduced pressure. Water was added to the residue, extraction was performed with AcOEt, and the organic layer was dried with Na2SO4 and then filtered and concentrated. The residue was purified by silica gel column chromatography (n-hexane/AcOEt=1/1) to obtain 6-bromomethyl-3,5-dimethyl-4-methoxymethoxy-2H-pyran-2-one.

후처리

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. additionWater was added to the residue, extraction
  3. dry with materialthe organic layer was dried with Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (n-hexane/AcOEt=1/1)

출처 및 근거

ORD 기록
ord-cf7f029ff12b4c058965df3a2b7b11e3
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06589984B1

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