Phosphorus oxychloride → Ethyl 5-Hydroxy-4-Methyl-7-(3-Methyl-2-Octyl)-Coumarin-3-Propionate

HRID 1112114

反応式

HRID 1112114 の反応式
[CH3:1][CH:2]([CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:3]([C:5]1[CH:6]=[C:7]([OH:12])[CH:8]=[C:9]([CH:11]=1)[OH:10])[CH3:4].[C:18]([CH:21]([CH2:27][CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])[C:22](OCC)=[O:23])(=O)[CH3:19].P(Cl)(Cl)(Cl)=O>>[OH:10][C:9]1[CH:11]=[C:5]([CH:3]([CH:2]([CH3:1])[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH3:4])[CH:6]=[C:7]2[C:8]=1[C:18]([CH3:19])=[C:21]([CH2:27][CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])[C:22](=[O:23])[O:12]2

参加物

4

反応物 3

HCID 24813Phosphorus oxychlorideHCID 73915Diethyl 2-acetylglutarateHCID 2581765-(3-Methyloctan-2-yl)benzene-1,3-diol

生成物 1

HCID 22765004Ethyl 5-Hydroxy-4-Methyl-7-(3-Methyl-2-Octyl)-Coumarin-3-Propionate

実験手順

A mixture of 262 g. (1.109 mole) of 5-(3-methyl-2-octyl)resorcinol, 283 g. (1.23 mole) of diethyl α-acetylglutarate, and 170 g. (1.11 mole) of phosphorus oxychloride protected from atmospheric moisture is stirred at room temperature for 12 days. The mixture is taken up in benzene-ether and the solution is washed several times with water, aqueous sodium bicarbonate, water and dried over anhydrous magnesium sulfate. After removal of the solvent, 441 g. of an oil is obtained, which solidifies on standing.

後処理

  1. additionA mixture of 262 g
  2. washthe solution is washed several times with water, aqueous sodium bicarbonate, water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customAfter removal of the solvent, 441 g
  5. customof an oil is obtained

出典と根拠

ORDレコード
ord-5cd16492be3548a8a610fa0336f0d8bd
出典データセット
uspto-grants-1978_10
特許番号
US04120873

関連ノート

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