Ethyl bromoacetate → HCID 21986425、化合物

HRID 9630ノート

反応式

HRID 9630 の反応式
[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([CH3:9])[C:6]([OH:10])=[C:5]([CH3:11])[CH:4]=1.Br[CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15].C(=O)([O-])[O-].[Cs+].[Cs+]>C(#N)C>[CH2:17]([O:16][C:14](=[O:15])[CH2:13][O:10][C:6]1[C:5]([CH3:11])=[CH:4][C:3]([CH2:2][OH:1])=[CH:8][C:7]=1[CH3:9])[CH3:18]

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 10796Cesium carbonateHCID 2786604-(hydroxymethyl)-2,6-dimethylphenol

生成物 1

HCID 21986425HCID 21986425、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 4-(hydroxymethyl)-2,6-dimethylphenol (P. Claus et al., Monatsh. Chem. 1972, 103(4), 1178–1193) (1.9 g) in acetonitrile (50 ml) was treated with ethyl bromoacetate (2.17 g) and caesium carbonate (4.24 g) and the mixture stirred at room temperature overnight. The solution was concentrated and the residue partitioned between ethyl acetate and water. The organic layer was collected, dried over magnesium sulfate and filtered. The filtrate was concentrated to give the title compound as a yellow oil.

後処理

  1. concentrationThe solution was concentrated
  2. customthe residue partitioned between ethyl acetate and water
  3. customThe organic layer was collected
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-42f38fc69f714700a45eeb1a3594703c
出典データセット
uspto-grants-2006_08
特許番号
US07091237B2

反応ノート

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