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

HRID 1019329

反応式

HRID 1019329 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 86758367HCID 86758367、化合物触媒HCID 62781,1,1-Trichloroethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-19ed3d7c5f8940d19128299bfcfcf4cd
出典データセット
uspto-grants-2002_11
特許番号
US06486338B1

関連ノート

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