Water → 4-[4-(Methacryloyloxy)butoxy]benzenecarboxylic acid

HRID 1019329

반응식

HRID 1019329 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1.[C:16](O)(=[O:20])[C:17]([CH3:19])=[CH2:18].C1(C)C=CC(S(O)(=O)=O)=CC=1.O>ClC(Cl)(Cl)C.C(C1CC(=CN(C)C)C=C(C(C)(C)C)C=1O)(C)(C)C>[C:16]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1)(=[O:20])[C:17]([CH3:19])=[CH2:18]

참가 물질

7

반응물 4

HCID 962WaterHCID 4093Methacrylic AcidHCID 6101p-Toluenesulfonic acidHCID 152185964-(4-Hydroxybutoxy)benzoic acid

생성물 1

HCID 37201354-[4-(Methacryloyloxy)butoxy]benzenecarboxylic acid수율 60%

시약·촉매·용매 2

HCID 86758367HCID 86758367, 화합물촉매HCID 62781,1,1-Trichloroethane용매

실험 절차

A solution of 282 g of 4-(4′-hydroxybutoxy)benzoic acid (1.34 mol), 325 ml of freshly distilled methacrylic acid (3.35 mol), 0.3 g of 2,6 di-tert-butyl-4-(dimethylaminomethylene)phenol (Ethanox® 703) and 23.7 g of p-toluenesulfonic acid in 1.1 l of 1,1,1-trichloroethane was refluxed for 10 hours on a water separator. The reaction mixture was cooled to 60° C.-70° C. and stirred into 2.51 of petroleum ether, and the precipitate was filtered off. After washing with petroleum ether, the precipitate was dried under reduced pressure at room temperature for 24 hours, giving 223.7 g of 4-(4′-methacryloxybutoxy)benzoic acid (yield 60%).

후처리

  1. temperatureThe reaction mixture was cooled to 60° C.-70° C.
  2. filtrationthe precipitate was filtered off
  3. washAfter washing with petroleum ether
  4. customthe precipitate was dried under reduced pressure at room temperature for 24 hours

출처 및 근거

ORD 기록
ord-19ed3d7c5f8940d19128299bfcfcf4cd
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06486338B1

연결된 노트

불러오는 중…