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

Water → 2,3-Difluoro-5-hydroxybenzoic acid

HRID 1051576
노트
인쇄 미리보기

반응식

HRID 1051576 반응식
O.O.O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[F:22][C:23]1[C:31]([F:32])=[CH:30][C:29]([O:33][Si](C(C)C)(C(C)C)C(C)C)=[CH:28][C:24]=1[C:25]([OH:27])=[O:26].O>O1CCCC1>[F:22][C:23]1[C:31]([F:32])=[CH:30][C:29]([OH:33])=[CH:28][C:24]=1[C:25]([OH:27])=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 11726816Tetrabutylammonium Fluoride TrihydrateHCID 848208732,3-Difluoro-5-(triisopropylsilyloxy)benzoic acid

생성물 1

HCID 265967652,3-Difluoro-5-hydroxybenzoic acid수율 95.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Tetrabutylammonium fluoride trihydrate (191 g, 731.8 mmol) was added in portions to a solution of 2,3-difluoro-5-(triisopropylsilyloxy)benzoic acid (99.13 g, 300.0 mmol) in tetrahydrofuran (500 mL), and the resulting mixture stirred overnight at room temperature. The reaction mixture was poured into water (1000 mL) and extracted with ethyl acetate (2×500 mL). The combined organic layers were washed with brine (2×500 mL), dried over anhydrous sodium sulfate, filtered, and concentrated under vacuum to afford 2,3-difluoro-5-hydroxybenzoic acid (50 g, 95%) as a light yellow solid. MS (ESI, neg. anion) m/z 173 [M−H]−.

후처리

  1. extractionextracted with ethyl acetate (2×500 mL)
  2. washThe combined organic layers were washed with brine (2×500 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-a451b73a7ca346ab8b3dfb3a9aaf9b1a
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388161B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트