Hydrochloric Acid → (E)-2-(3-Chloroprop-1-en-1-yl)-1,4-difluorobenzene

HRID 1644408노트

반응식

HRID 1644408 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1/[CH:9]=[CH:10]/[CH2:11]O.[ClH:13]>O1CCOCC1>[Cl:13][CH2:11]/[CH:10]=[CH:9]/[C:3]1[CH:4]=[C:5]([F:8])[CH:6]=[CH:7][C:2]=1[F:1]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 667739363-(2,5-Difluorophenyl)prop-2-en-1-ol2회

생성물 1

HCID 11608064(E)-2-(3-Chloroprop-1-en-1-yl)-1,4-difluorobenzene수율 89%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

A mixture of (2E)-3-(2,5-difluorophenyl)prop-2-en-1-ol (Intermediate 70, 700 mg, 4.12 mmol), 1,4-dioxane (5 mL), and hydrochloric acid (12.1 M, 1 mL) was heated in the microwave at 100° C. for 3 hours. It was concentrated to dryness under reduced pressure, the residue taken up in ethyl acetate (10 mL), washed with water (1×10 mL), saturated sodium bicarbonate solution, brine and dried over sodium sulfate. The solvent was removed under reduced pressure to give 688 mg (89% yield) of product as a yellow oil.

후처리

  1. concentrationIt was concentrated to dryness under reduced pressure
  2. washwashed with water (1×10 mL), saturated sodium bicarbonate solution, brine
  3. dry with materialdried over sodium sulfate
  4. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-9eb8c6f0374149daa4e9d08b85e6baff
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08124602B2

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