Hydrochloric Acid → 3-(2-Bromo-4,5-difluorophenoxy)propanoic acid

HRID 1363193노트

반응식

HRID 1363193 반응식
[OH-].[Na+].[Br:3][C:4]1[CH:9]=[C:8]([F:10])[C:7]([F:11])=[CH:6][C:5]=1[OH:12].Br[CH2:14][CH2:15][C:16]([OH:18])=[O:17].Cl>O>[Br:3][C:4]1[CH:9]=[C:8]([F:10])[C:7]([F:11])=[CH:6][C:5]=1[O:12][CH2:14][CH2:15][C:16]([OH:18])=[O:17]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 115533-Bromopropionic acidHCID 14798Sodium HydroxideHCID 27362882-Bromo-4,5-difluorophenol

생성물 1

HCID 669704713-(2-Bromo-4,5-difluorophenoxy)propanoic acid수율 66%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
100 °C

실험 절차

A solution of 1.68 g of NaOH (42 mmol) in 5 mL of water was added slowly to the suspension of 2.29 mL (20 mmol) 2-bromo-4,5-difluorophenol and 3.07 g (20 mmol) 3-bromopropionic acid. The mixture was heated at 100° C. in an oil bath for 5 hours, and then allowed to cool to room temperature. Water was added to completely dissolve any solid material and the reaction mixture was made acidic with concentrated HCl. The product was extracted into ether (3 times), and the combined organic layers was dried over Na2SO4 and evaporated to give 3.7 g (66%) of the title compound as a light brown solid. 1H NMR (300 MHz, CDCl3): δ 7.4 (t, 1H), 6.8 (q, 1H), 4.3 (t, 2H), 2.9 (t, 2H).

후처리

  1. temperatureto cool to room temperature
  2. dissolutionto completely dissolve any solid material
  3. extractionThe product was extracted into ether (3 times)
  4. dry with materialthe combined organic layers was dried over Na2SO4
  5. customevaporated

출처 및 근거

ORD 기록
ord-60e853fb7e654056ba69a9ba2409c65e
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07884109B2

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