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Water → 3-Benzylpyrrolylmethyl 3-(4-chlorophenoxy)-2,2-dimethylcyclopropanecarboxylate

HRID 903799
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HRID 903799 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([O:6][CH:7]2[CH:9]([C:10]([OH:12])=[O:11])[C:8]2([CH3:14])[CH3:13])=[CH:4][CH:3]=1.S(Cl)(Cl)=O.[CH2:21]([C:28]1[CH:32]=[CH:31][NH:30][C:29]=1[CH2:33]O)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.O>CN(C=O)C.C1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH:7]2[CH:9]([C:10]([O:12][CH2:33][C:29]3[NH:30][CH:31]=[CH:32][C:28]=3[CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[O:11])[C:8]2([CH3:13])[CH3:14])=[CH:15][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 24386Thionyl ChlorideHCID 203049613-(4-Chlorophenoxy)-2,2-dimethylcyclopropanecarboxylic acidHCID 543430813-Benzyl-1-pyrrolylmethanol

생성물 1

HCID 233351473-Benzylpyrrolylmethyl 3-(4-chlorophenoxy)-2,2-dimethylcyclopropanecarboxylate

시약·촉매·용매 2

HCID 6228
Dimethylformamide
촉매
HCID 241Benzene용매

실험 절차

A mixture of 3-(4-chlorophenoxy)-2,2-dimethylcyclopropanecarboxylic acid (0.95 g, 3.95 mmol), thionyl chloride (0.342 ml, 4.74 mmol) and DMF (several drops) in 50 ml benzene is stirred at RT for 2 days. The solvent and excess thionyl chloride are evaporated under reduced pressure. The resulting acid chloride is dissolved in 50 ml benzene, and 3-benzylpyrrolylmethyl alcohol (3.95 mmol) and 0.482 g 4-dimethtylaminopyridine (3.95 mmol) are added. The mixture is left at 25° for 18 hours and then heated under reflux for 2 hours. The mixture is then poured into water and extracted with ether. The organic phase is washed with dilute HCl, sat. NaHCO3, water and brine, dried and concentrated under vacuum. The crude product is purified by preparative TLC developing with 20% ethyl acetate/hexane to yield 3-benzylpyrrolylmethyl 3-(4-chlorophenoxy)-2,2-dimethylcyclopropanecarboxylate (A; R is hydrogen, X=X' is methyl, W is oxygen, R1 is 4-chlorophenyl).

후처리

  1. customThe solvent and excess thionyl chloride are evaporated under reduced pressure
  2. dissolutionThe resulting acid chloride is dissolved in 50 ml benzene
  3. waitThe mixture is left at 25° for 18 hours
  4. temperatureheated
  5. temperatureunder reflux for 2 hours
  6. extractionextracted with ether
  7. washThe organic phase is washed with dilute HCl, sat. NaHCO3, water and brine
  8. customdried
  9. concentrationconcentrated under vacuum
  10. customThe crude product is purified by preparative TLC

출처 및 근거

ORD 기록
ord-cca25ef4cd0d40f89edff0ba43c0a1de
출처 데이터셋
uspto-grants-1980_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04229352

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