4-Hydroxybenzyl Alcohol → 6-[4-(Hydroxymethyl)phenoxy]hexyl prop-2-enoate

HRID 28315

반응식

HRID 28315 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][OH:7])=[CH:4][CH:3]=1.[C:10]([O:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]I)(=[O:13])[CH:11]=[CH2:12].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[C:10]([O:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][OH:7])=[CH:4][CH:3]=1)(=[O:13])[CH:11]=[CH2:12]

참가 물질

5

반응물 3

HCID 1254-Hydroxybenzyl AlcoholHCID 11430Potassium CarbonateHCID 11289038Acrylic acid 6-iodohexyl ester

생성물 1

HCID 234484226-[4-(Hydroxymethyl)phenoxy]hexyl prop-2-enoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

A mixture consisting of 2.48 g of 4-hydroxybenzylalcohol, 5.64 g of 6-iodohexyl acrylate, and 2.76 g of potassium carbonate in 50 ml of DMF was stirred under nitrogen atmosphere for 3 h at 60° C. After being cooled to room temperature the reaction mixture was quenched with 100 ml 3N HCl and extracted with diethylether (2×100 ml). The combined ether extracts were washed with saturated NaCl solution, dried over sodium sulphate and concentrated to dryness to give 5.3 g of nearly pure 4-(6-acryloyloxyhexyloxy)benzylalcohol as a beige heavy oil.

후처리

  1. temperatureAfter being cooled to room temperature the reaction mixture
  2. customwas quenched with 100 ml 3N HCl
  3. extractionextracted with diethylether (2×100 ml)
  4. washThe combined ether extracts were washed with saturated NaCl solution
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-baca2d09bcd849169359f86b1ed8d54e
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07419620B2

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