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

Trifluoroacetic anhydride → 2-Fluoro-3-methoxy-5-methylbenzenethiol

HRID 591443
노트
인쇄 미리보기

반응식

HRID 591443 반응식
[F:1][C:2]1[C:7]([S:8](C)=O)=[CH:6][C:5]([CH3:11])=[CH:4][C:3]=1[O:12][CH3:13].C(OC(C(F)(F)F)=O)(C(F)(F)F)=O>CC#N>[F:1][C:2]1[C:3]([O:12][CH3:13])=[CH:4][C:5]([CH3:11])=[CH:6][C:7]=1[SH:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 897676932-Fluoro-1-methoxy-5-methyl-3-(methylsulfinyl)benzene

생성물 1

HCID 897676722-Fluoro-3-methoxy-5-methylbenzenethiol수율 51.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
0 °C

실험 절차

To a mixture of 2-fluoro-1-methoxy-5-methyl-3-(methylsulfinyl)benzene (486 mg) and CH3CN (20 mL) was added TFAA (1.02 mL) at 0° C. The mixture was stirred at 0° C. for 1 h, and concentrated in vacuo. The residue was dissolved in a mixture of MeOH (3.5 mL) and TEA (3.5 mL) at 0° C. The solution was stirred at room temperature for 1 h, and concentrated in vacuo. The residue was diluted with saturated aqueous NH4Cl, and the mixture was extracted with EtOAc. The organic layer was extracted with 1N NaOH. The aqueous layer was acidified with 1N HCl and extracted with EtOAc. The combined organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo to give the title compound (214 mg).

후처리

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in a mixture of MeOH (3.5 mL) and TEA (3.5 mL) at 0° C
  3. stirringThe solution was stirred at room temperature for 1 h
  4. concentrationconcentrated in vacuo
  5. additionThe residue was diluted with saturated aqueous NH4Cl
  6. extractionthe mixture was extracted with EtOAc
  7. extractionThe organic layer was extracted with 1N NaOH
  8. extractionextracted with EtOAc
  9. washThe combined organic layer was washed with brine
  10. dry with materialdried over MgSO4
  11. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ea7f7ee883d241b3b60d95f0f3c2670a
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238639B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트