Sodium hydride → Methyl [4-(4-methoxybenzoyl)-2-methylphenoxy]acetate

HRID 1649956ノート

反応式

HRID 1649956 の反応式
[OH:1][C:2]1[CH:17]=[CH:16][C:5]([C:6]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)=[O:7])=[CH:4][C:3]=1[CH3:18].[H-].[Na+].Br[CH2:22][C:23]([O:25][CH3:26])=[O:24]>CN(C=O)C>[CH3:15][O:14][C:11]1[CH:12]=[CH:13][C:8]([C:6]([C:5]2[CH:16]=[CH:17][C:2]([O:1][CH2:22][C:23]([O:25][CH3:26])=[O:24])=[C:3]([CH3:18])[CH:4]=2)=[O:7])=[CH:9][CH:10]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 60984Methyl bromoacetateHCID 13966818HCID 13966818、化合物

生成物 1

HCID 13966816Methyl [4-(4-methoxybenzoyl)-2-methylphenoxy]acetate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

50 g of 4-hydroxy-3-methyl-4'-methoxybenzophenone (R. Martin et al. Monatsh. Chemie 110, 1057-1066 (1979)) are dissolved in 200 ml of dry DMF and, under N2, 9 g of a 55% dispersion of sodium hydride in mineral oil are cautiously added. Then, while stirring, 19.5 ml of methyl bromoacetate are added dropwise, and the mixture is left to stand at room temperature overnight. The precipitated salt is filtered off with suction, and the filtrate is concentrated in vacuo. The residue is taken up in ethyl acetate, and the solution is washed with sodium bicarbonate solution and water. The organic phase is dried over magnesium sulfate, and the solvent is removed in vacuo. The residue is triturated with ether, filtered off with suction and dried.

後処理

  1. waitthe mixture is left
  2. filtrationThe precipitated salt is filtered off with suction
  3. concentrationthe filtrate is concentrated in vacuo
  4. washthe solution is washed with sodium bicarbonate solution and water
  5. dry with materialThe organic phase is dried over magnesium sulfate
  6. customthe solvent is removed in vacuo
  7. customThe residue is triturated with ether
  8. filtrationfiltered off with suction
  9. customdried

出典と根拠

ORDレコード
ord-b62a71e5efb74246af51a330d376a20e
出典データセット
uspto-grants-1990_05
特許番号
US04922015

反応ノート

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