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

HRID 591560ノート

反応式

HRID 591560 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-75d09aaaaa54434dad06955e30bff04f
出典データセット
uspto-grants-2016_01
特許番号
US09238639B2

反応ノート

読み込み中…