1,4-Butanediol → 4-Hydroxybutyl 3-(ethyl-4-hydroxybutoxyphosphinyl)-2-methylpropionate

HRID 1028259노트

반응식

HRID 1028259 반응식
[CH2:1]([P:3]([OH:11])([CH2:5][CH:6]([CH3:10])[C:7]([OH:9])=[O:8])=[O:4])[CH3:2].[CH2:12](O)[CH2:13][CH2:14][CH2:15][OH:16]>C1(C)C=CC=CC=1>[CH2:1]([P:3]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][OH:16])([CH2:5][CH:6]([CH3:10])[C:7]([O:9][CH2:12][CH2:13][CH2:14][CH2:15][OH:16])=[O:8])=[O:4])[CH3:2]

참가 물질

4

반응물 2

HCID 80641,4-ButanediolHCID 462165003-(Ethylhydroxyphosphinyl)-2-methylpropionic acid

생성물 1

HCID 866573094-Hydroxybutyl 3-(ethyl-4-hydroxybutoxyphosphinyl)-2-methylpropionate수율 92%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

540 g (3.0 mol) of 3-(ethylhydroxyphosphinyl)-2-methylpropionic acid (produced as in Example 17) are at 80° C. dissolved in 400 ml of toluene and admixed with 594 g (6.6 mol) of 1,4-butanediol and esterified at about 100° C. in a distillation apparatus equipped with water trap during 4 h. On completion of the esterification the toluene is removed in vacuo to leave 894 g (92% of theory) of 4-hydroxybutyl 3-(ethyl-4-hydroxybutoxyphosphinyl)-2-methylpropionate as colorless oil.

후처리

  1. customare at 80° C.
  2. customesterified at about 100° C. in a distillation apparatus
  3. customequipped with water trap during 4 h
  4. customOn completion of the esterification the toluene is removed in vacuo

출처 및 근거

ORD 기록
ord-bcee0e373d8d4d26a84da10a93dc0b7d
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08735477B2

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