Methylparaben → Methyl 4-(tetradecyloxy)benzoate

HRID 247911

반응식

HRID 247911 반응식
[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32]>CC(=O)CC>[CH3:1][O:2][C:3](=[O:11])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH3:19])=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 7456MethylparabenHCID 8208Myristyl bromideHCID 11430Potassium Carbonate

생성물 1

HCID 3312490Methyl 4-(tetradecyloxy)benzoate

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A mixture of 150 g methyl-4-hydroxybenzoate, 1.5 L 2-butanone, 272.5 g potassium carbonate and 293 ml 1-bromotetradecane is heated at reflux for 66 hours. The reaction is cooled to room temperature, filtered, the filtrate concentrated in vacuo and the residue recrystallized from methylene chloride/hexane to give 258.8 g of the desired product. MP 56°-58° C.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 66 hours
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated in vacuo
  5. customthe residue recrystallized from methylene chloride/hexane

출처 및 근거

ORD 기록
ord-6b25509aea6d47dfb14ef8b085b63220
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05208247

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