Propylene Glycol → 2-Chloromethyl-4-methyl-2-(2,5-dimethylphenyl)-[1,3]dioxolane

HRID 1866791ノート

反応式

HRID 1866791 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)[CH:14]([OH:16])[CH3:15]>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][CH:14]([CH3:15])[CH2:13][O:4]1

参加物

4

反応物 2

HCID 1030Propylene GlycolHCID 23636932-Chloro-1-(2,5-dimethylphenyl)ethan-1-one

生成物 1

HCID 578106322-Chloromethyl-4-methyl-2-(2,5-dimethylphenyl)-[1,3]dioxolane

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A mixture of 36.5 g [0.2 mol] of 2-chloro-1-(2,5-dimethylphenyl)ethanone, 22.8 g [0.3 mol] of propylene glycol, 3.6 g [0.02 mol] of p-TsOH hydrate and 150 ml of xylene is heated to boiling with a water trap for about 1.5 hours. Part of the xylene is then distilled off, and the reaction mixture is extracted at room temperature twice with 100 ml of water each time. The organic phase is dried over sodium sulfate and concentrated in vacuo, and volatiles are distilled off up to about 50° C./0.2 mbar. 39.65 g of an orange-colored oil remain with, according to GC, 93.0% product (76.7% of theory).

後処理

  1. temperatureis heated
  2. distillationPart of the xylene is then distilled off
  3. extractionthe reaction mixture is extracted at room temperature twice with 100 ml of water each time
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. concentrationconcentrated in vacuo, and volatiles
  6. distillationare distilled off up to about 50° C./0.2 mbar

出典と根拠

ORDレコード
ord-02b7b4f943c348c3a44f3924165a94df
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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