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

HRID 1866791노트

반응식

HRID 1866791 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-02b7b4f943c348c3a44f3924165a94df
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07629476B2

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