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Epichlorohydrin → HCID 20212125, 화합물

HRID 1906519
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HRID 1906519 반응식
[I:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[OH:12].[H-].[Na+].[CH2:15]([CH:17]1[O:19][CH2:18]1)Cl>CN(C=O)C>[I:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:10])([F:11])[F:9])=[CH:4][C:3]=1[O:12][CH2:15][CH:17]1[CH2:18][O:19]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7835EpichlorohydrinHCID 24758Sodium hydrideHCID 138235382-Iodo-5-(trifluoromethyl)phenol

생성물 1

HCID 20212125HCID 20212125, 화합물수율 86%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

A sample of 20 g (0.069 mole) of 2-iodo-5-trifluoromethylphenol was added in portions to a suspension of 0.07 mole of NaH (from 3.36 g of 50% NaH which had been washed free of oil with hexane) in 150 ml of dry DMF under N2. When gas evolution had ceased, a 27 ml (0.347 mole) sample of epichlorohydrin was added dropwise at 5° C. The mixture was heated at 60° C. for 3 hr and allowed to stand at 25° C. for 16 hr. A precipitate was removed by filtration. The filtrate was concentrated to dryness in vacuo. The residue was taken up in ether, washed with water and brine, dried (K2CO3) and the solvent evaporated in vacuo to give 20.4 g (86% yield) of [(2-iodo-5-trifluoromethylphenoxy)methyl]oxirane as an oil.

후처리

  1. customA precipitate was removed by filtration
  2. concentrationThe filtrate was concentrated to dryness in vacuo
  3. washwashed with water and brine
  4. dry with materialdried (K2CO3)
  5. customthe solvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-91cbc5e5b04a4ed185c800e5fcaa4970
출처 데이터셋
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04652584

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