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

HRID 1866789노트

반응식

HRID 1866789 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)[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 7237O-Xylene용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-60551379df194a8fb0ccfd64a74a5a26
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07629476B2

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