홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → 3-Bromo-6-(2,2-difluoroethoxy)-2-methylpyridine

HRID 623537
노트
인쇄 미리보기

반응식

HRID 623537 반응식
[Br:1][C:2]1[C:3]([CH3:9])=[N:4][C:5](Br)=[CH:6][CH:7]=1.[F:10][CH:11]([F:14])[CH2:12][OH:13].CC(C)([O-])C.[K+].O>C1COCC1>[Br:1][C:2]1[C:3]([CH3:9])=[N:4][C:5]([O:13][CH2:12][CH:11]([F:14])[F:10])=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 1361872,2-Difluoroethan-1-olHCID 27629463,6-Dibromo-2-methylpyridineHCID 23665647Potassium tert-butoxide

생성물 1

HCID 874266193-Bromo-6-(2,2-difluoroethoxy)-2-methylpyridine수율 97%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
70 °C

실험 절차

To a mixture of 3,6-dibromo-2-methylpyridine (2.00 g, 7.97 mmol) and 2,2-difluoroethanol (981 mg, 12.0 mmol) in THF (100 mL) is added potassium tert-butoxide (1.34 g, 12.0 mmol), and the mixture is stirred at 70° C. for 12 hours. After cooling to room temperature, the resulting mixture is poured to water (200 mL). The aqueous layer is extracted with ethyl acetate (200 mL×2). The organic layer is dried over sodium sulfate and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (8:1) to give 1.94 g (97% yield) of the title compound as colorless oil.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionThe aqueous layer is extracted with ethyl acetate (200 mL×2)
  3. dry with materialThe organic layer is dried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (8:1)

출처 및 근거

ORD 기록
ord-372c676eed334e82bd7d0306c2966254
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09302991B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트