Ethanol → 5-(3-chloro-4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one

HRID 655460ノート

反応式

HRID 655460 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:10](=[O:17])[C:11]#[C:12][C:13](O)([CH3:15])[CH3:14])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].C(NCC)C.C([OH:25])C>>[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2[O:17][C:13]([CH3:14])([CH3:15])[C:12](=[O:25])[CH:11]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9]

参加物

4

反応物 3

HCID 702Ethanol2 回HCID 8021DiethylamineHCID 593547741-(3-Chloro-4-methoxyphenyl)-4-hydroxy-4-methylpent-2-yn-1-one

生成物 1

HCID 593548485-(3-chloro-4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one収率 100%

実験手順

To a stirred solution of 1-(3-chloro-4-methoxyphenyl)-4-hydroxy-4-methylpent-2-yn-1-one (0.7 g, 2.75 mmol) in ethanol (5 mL), a solution of diethyl amine (0.20 g, 2.75 mmol) in EtOH (7 mL) was added dropwise at RT. The reaction mixture was then stirred for additional 30 min. The ethanol was removed, and the reaction mixture diluted with EtOAc (10 mL). The combined organic layers were then washed with water (5 mL) and brine (5 mL), dried over Na2SO4, filtered, and concentrated in vacuo to afford 5-(3-chloro-4-methoxyphenyl)-2,2-dimethylfuran-3(2H)-one (0.7 g, 100%) as a semi solid.

後処理

  1. customThe ethanol was removed
  2. additionthe reaction mixture diluted with EtOAc (10 mL)
  3. washThe combined organic layers were then washed with water (5 mL) and brine (5 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-95620ccfaa3a45dca29a9e35245aec38
出典データセット
uspto-grants-2011_12
特許番号
US08071595B2

反応ノート

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