Ethylene Glycol → 2-Chloromethyl-2-(2,5-dimethylphenyl)-[1,3]dioxolane

HRID 1866789ノート

反応式

HRID 1866789 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].[CH2:13](O)[CH2:14][OH:15].[Na+].[Cl-]>C1(C)C(C)=CC=CC=1.O>[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:15][CH2:14][CH2:13][O:4]1

参加物

6

反応物 3

HCID 174Ethylene GlycolHCID 5234Sodium ChlorideHCID 23636932-Chloro-1-(2,5-dimethylphenyl)ethan-1-one

生成物 1

HCID 578106302-Chloromethyl-2-(2,5-dimethylphenyl)-[1,3]dioxolane収率 80.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7237O-Xylene溶媒2 回

実験手順

A mixture of 18.3 g [0.1 mol] of 2-chloro-1-(2,5-dimethylphenyl)ethanone, 12.6 g [0.2 mol] of ethylene glycol, 1.9 g [0.01 mol] of p-TsOH hydrate and 100 ml of xylene is heated to boiling with a water trap for about 3 hours. 40 ml of water and 20 ml of saturated aqueous NaCl solution are then added to the reaction mixture at room temperature. After addition of 20 ml of xylene, the organic phase is separated off and extracted with 20 ml each of water and saturated aqueous NaCl solution. The organic phase is dried over sodium sulfate and concentrated in vacuo. 18.35 g of oil result with, according to GC, 95.3% product (77.2% of theory).

後処理

  1. temperatureis heated
  2. customthe organic phase is separated off
  3. extractionextracted with 20 ml each of water and saturated aqueous NaCl solution
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-60551379df194a8fb0ccfd64a74a5a26
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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