Dimethylformamide → Methyl 4-((3-fluoro-5-methoxyphenyl)sulfanyl)-3-oxobutanoate

HRID 591560노트

반응식

HRID 591560 반응식
Cl[CH2:2][C:3](=[O:9])[CH2:4][C:5]([O:7][CH3:8])=[O:6].[F:10][C:11]1[CH:12]=[C:13]([SH:19])[CH:14]=[C:15]([O:17][CH3:18])[CH:16]=1.CN(C=O)C>O>[F:10][C:11]1[CH:12]=[C:13]([S:19][CH2:2][C:3](=[O:9])[CH2:4][C:5]([O:7][CH3:8])=[O:6])[CH:14]=[C:15]([O:17][CH3:18])[CH:16]=1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 36240Methyl 4-chloroacetoacetateHCID 897677523-Fluoro-5-methoxybenzenethiol

생성물 1

HCID 89768091Methyl 4-((3-fluoro-5-methoxyphenyl)sulfanyl)-3-oxobutanoate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of methyl 4-chloroacetoacetate (1.871 mL), K2OC3 (2.210 g), 3-fluoro-5-methoxybenzenethiol (2.3 g) and DMF (30 mL) was stirred at room temperature for 1 h. The mixture was poured into water and extracted with EtOAc. The organic layer was separated, washed successively with water and brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (2.87 g).

후처리

  1. extractionextracted with EtOAc
  2. customThe organic layer was separated
  3. washwashed successively with water and brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel column chromatography (EtOAc/hexane)

출처 및 근거

ORD 기록
ord-75d09aaaaa54434dad06955e30bff04f
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238639B2

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