2-Chloroethanol → 2-[4'-(2",4"-Dichlorophenoxy)-phenoxy]-propionic acid 2-chloroeth-1-yl ester

HRID 903379노트

반응식

HRID 903379 반응식
[Cl:1][C:2]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:16]=[CH:15][C:8]([O:9][CH:10]([CH3:14])[C:11](Cl)=[O:12])=[CH:7][CH:6]=1.C(O)(=O)CC.S(Cl)(Cl)=O.[CH2:31]([Cl:34])[CH2:32][OH:33]>C1(C)C=CC=CC=1.C(N(CC)CC)C>[Cl:34][CH2:31][CH2:32][O:33][C:11](=[O:12])[CH:10]([O:9][C:8]1[CH:15]=[CH:16][C:5]([O:4][C:3]2[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:2]=2[Cl:1])=[CH:6][CH:7]=1)[CH3:14]

참가 물질

7

반응물 4

HCID 342-ChloroethanolHCID 1032Propionic AcidHCID 24386Thionyl ChlorideHCID 129429952-[4-(2,4-Dichlorophenoxy)phenoxy]propanoyl chloride

생성물 1

HCID 545418052-[4'-(2",4"-Dichlorophenoxy)-phenoxy]-propionic acid 2-chloroeth-1-yl ester

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 8471Triethylamine용매

실험 절차

A solution of 0.06 mol=20.73 g of 2-[4'-(2",4"-dichlorophenoxy)phenoxy]-propionic acid chloride, prepared from 2-[4'-2",4"-dichlorophenoxy)phenoxy]-propionic acid and thionyl chloride, in 60 ml absolute toluene was added dropwise at room temperature to a solution of 0.06 mol=4.83 g of ethylene chlorohydrin (2-chloroethanol) and 0.06 mol=6.06 g of triethylamine in 60 ml absolute toluene. After the addition, stirring of the mixture was continued for 1 hour at 50° C., the precipitated triethylamine chloride was filtered off, and the filtrate was washed with dilute sodium hydroxide solution and with water. The toluene solution was dried over sodium sulfate and the solvent was distilled off under reduced pressure. 21.25 g=91% of the theory of 2-[4'-(2",4"-dichlorophenoxy)-phenoxy]-propionic acid 2-chloroeth-1-yl ester were obtained having a refractive index nD24 of 1.5672. ##STR13##

후처리

  1. additionAfter the addition
  2. filtrationthe precipitated triethylamine chloride was filtered off
  3. washthe filtrate was washed with dilute sodium hydroxide solution and with water
  4. dry with materialThe toluene solution was dried over sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-1385d9537f6846bdb3550df61e6ae484
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04227009

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