Water → 2-Chloromethyl-5,5-dimethyl-2-(2,5-dimethylphenyl)-[1,3]dioxane

HRID 1866787ノート

反応式

HRID 1866787 の反応式
[Cl:1][CH2:2][C:3]([C:5]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:6]=1[CH3:12])=[O:4].[CH3:13][C:14]([CH3:19])([CH2:17]O)[CH2:15][OH:16].O>C1(C)C(C)=CC=CC=1>[Cl:1][CH2:2][C:3]1([C:5]2[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:6]=2[CH3:12])[O:16][CH2:15][C:14]([CH3:19])([CH3:17])[CH2:13][O:4]1

参加物

5

反応物 3

HCID 962Water2 回HCID 31344Neopentyl glycolHCID 23636932-Chloro-1-(2,5-dimethylphenyl)ethan-1-one

生成物 1

HCID 578106312-Chloromethyl-5,5-dimethyl-2-(2,5-dimethylphenyl)-[1,3]dioxane

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒2 回

実験手順

0.5 mol of 2-chloro-1-(2,5-dimethylphenyl)ethanone, 104 g [1 mol] of 2,2-dimethyl-1,3-propanediol (neopentyl glycol) and 9.5 g [0.05 mol] of p-TsOH hydrate are boiled in 500 ml of xylene with a water trap until the formation of water ceases (about 4 hours). 200 ml of water and 30 ml of xylene are added to the reaction mixture at room temperature. A better phase separation is achieved by adding 50 ml of saturated aqueous NaCl solution. The organic phase is then extracted again with 100 ml of water and 100 ml of saturated aqueous NaCl solution, dried and concentrated.

後処理

  1. customA better phase separation
  2. additionby adding 50 ml of saturated aqueous NaCl solution
  3. extractionThe organic phase is then extracted again with 100 ml of water and 100 ml of saturated aqueous NaCl solution
  4. customdried
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-80474765957f4da28dad361605b63493
出典データセット
uspto-grants-2009_12
特許番号
US07629476B2

反応ノート

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