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

HRID 1258340노트

반응식

HRID 1258340 반응식
[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]

참가 물질

4

반응물 3

HCID 702Ethanol2회HCID 8021DiethylamineHCID 593547741-(3-Chloro-4-methoxyphenyl)-4-hydroxy-4-methylpent-2-yn-1-one

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a5a476c1d7f64185b8affbc1dcddfa0f
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466148B2

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