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

HRID 1866787노트

반응식

HRID 1866787 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].[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

참가 물질

5

반응물 3

HCID 962Water2회HCID 31344Neopentyl glycolHCID 23636932-Chloro-1-(2,5-dimethylphenyl)ethan-1-one

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-80474765957f4da28dad361605b63493
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07629476B2

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