Ethyl bromoacetate → Ethyl 2-(4-acetyl-2-methylphenoxy)acetate

HRID 1909571

反応式

HRID 1909571 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][C:3]=1[CH3:11].Br[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15].C(=O)([O-])[O-].[Cs+].[Cs+]>C(#N)C>[C:8]([C:5]1[CH:6]=[CH:7][C:2]([O:1][CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:3]([CH3:11])[CH:4]=1)(=[O:10])[CH3:9]

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 10796Cesium carbonateHCID 701354'-Hydroxy-3'-methylacetophenone

生成物 1

HCID 21986544Ethyl 2-(4-acetyl-2-methylphenoxy)acetate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 1-(4-hydroxy-3-methylphenyl)ethanone (5 g, 33.3 mmol), ethyl 2-bromoacetate (1.1 eq.), and cesium carbonate (2 eq.) in acetonitrile (200 mL) was stirred at room temperature overnight. The acetonitrile was removed in vacuo, and the crude oil was dissolved in ethyl acetate (50 mL) and washed with 1M HCl (2×50 mL), water (2×50 mL), and brine (50 mL). The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo to obtain ethyl 2-(4-acetyl-2-methylphenoxy)acetate (683).

後処理

  1. customThe acetonitrile was removed in vacuo
  2. dissolutionthe crude oil was dissolved in ethyl acetate (50 mL)
  3. washwashed with 1M HCl (2×50 mL), water (2×50 mL), and brine (50 mL)
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-643e1ec6f4d74f45bb7fafa11fbbb248
出典データセット
uspto-grants-2013_12
特許番号
US08598374B2

関連ノート

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