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

Sodium borohydride → Ethyl {4-[9-(ethyloxy)-4-hydroxy-1-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-3-fluorophenyl}acetate

HRID 222436
노트
인쇄 미리보기

반응식

HRID 222436 반응식
[CH2:1]([O:3][C:4]1[C:12]2[C:11](=[O:13])[N:10]([C:14]3[CH:19]=[CH:18][C:17]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:16][C:15]=3[F:26])[C:9](=O)[C:8]=2[C:7]([OH:28])=[C:6]2[CH:29]=[CH:30][CH:31]=[CH:32][C:5]=12)[CH3:2].[BH4-].[Na+]>C1COCC1>[CH2:1]([O:3][C:4]1[C:12]2[C:11](=[O:13])[N:10]([C:14]3[CH:19]=[CH:18][C:17]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[CH:16][C:15]=3[F:26])[CH2:9][C:8]=2[C:7]([OH:28])=[C:6]2[CH:29]=[CH:30][CH:31]=[CH:32][C:5]=12)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4311764Sodium borohydride3회HCID 58012505Ethyl {4-[4-(ethyloxy)-9-hydroxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-3-fluorophenyl}acetate

생성물 1

HCID 58231483Ethyl {4-[9-(ethyloxy)-4-hydroxy-1-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-3-fluorophenyl}acetate수율 101.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of ethyl {4-[4-(ethyloxy)-9-hydroxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl]-3-fluorophenyl}acetate (2.50 g, 5.72 mmol) in THF (50 ml) under an argon atmosphere, was added sodium borohydride (0.217 g, 5.72 mmol) followed by borane THF complex solution (1.0M in THF, 5.72 ml, 5.72 mmol). This was stirred at room temperature for 2 hours. A further 5.72 mmol of sodium borohydride and borane THF complex was added to the reaction mixture and stirring continued for 2 hours. Finally, a further 2.86 mmol addition of sodium borohydride and borane THF complex was made and stirring continued for 1.5 hours until the reaction was complete. This was quenched with ethyl acetate (100 ml) and methanol (3 ml) then washed with 2N HCl (100 ml). The aqueous was re-extracted with ethyl acetate (200 ml). The combined organics were washed with brine (200 ml), dried over magnesium sulphate, filtered and evaporated to give the title compound as a pale yellow solid (2.45 g, 5.79 mmol).

후처리

  1. stirringstirring
  2. waitcontinued for 2 hours
  3. stirringstirring
  4. waitcontinued for 1.5 hours until the reaction
  5. customThis was quenched with ethyl acetate (100 ml) and methanol (3 ml)
  6. washthen washed with 2N HCl (100 ml)
  7. extractionThe aqueous was re-extracted with ethyl acetate (200 ml)
  8. washThe combined organics were washed with brine (200 ml)
  9. dry with materialdried over magnesium sulphate
  10. filtrationfiltered
  11. customevaporated

출처 및 근거

ORD 기록
ord-c92bf9c790674d8db3865294738c3db8
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08207213B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트