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

2-Cyclohexen-1-one → 3-(4-(Benzyloxy)phenyl)cyclohexanone

HRID 1713844
노트
인쇄 미리보기

반응식

HRID 1713844 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12](B(O)O)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.[C:64]1(=[O:70])[CH2:69][CH2:68][CH2:67][CH:66]=[CH:65]1.C(=O)([O-])O.[Na+]>O1CCOCC1.O>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH:66]2[CH2:67][CH2:68][CH2:69][C:64](=[O:70])[CH2:65]2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 135942-Cyclohexen-1-oneHCID 516892Sodium BicarbonateHCID 634876Binap, (A+-)-HCID 27343144-Benzyloxy-phenylboronic acid

생성물 1

HCID 594642333-(4-(Benzyloxy)phenyl)cyclohexanone수율 23%

시약·촉매·용매 1

HCID 21886435
1,4-Dioxane--water (1/1)
용매

실험 절차

[4-(Benzyloxy)phenyl]boronic acid (2 g, 8.77 mmol) was dissolved in dioxane/water (50 mL/5 mL) and Rh(acac)(C2H4)2 (68 mg, 0.26 mmol) and racemic BINAP (164 mg, 0.26 mmol) were added. The mixture was degassed 3 times and put under a nitrogen atmosphere. Cyclohexenone (1.02 mL, 10.52 mmol) was added to the yellow solution and the mixture heated at reflux overnight. The reaction mixture was cooled, saturated aqueous sodium hydrogen carbonate solution (50 mL) added, then extracted with EtOAc (2×100 mL). The organic extracts were washed with water (100 mL) and dried. Volatile material was removed by evaporation and purification by chromatography gave the title compound (565 mg, 23%) as a solid; 1H NMR δ1.65-1.69 (1H, m), 1.78-1.93 (2H, m), 1.99-2.04 (1H, m), 2.22-2.35 (2H, m), 2.39-2.43 (1H, m), 2.65 (1H, m), 2.90-2.96 (1H, m), 5.08 (2H, s), 6.96 (2H, d), 7.20 (2H, d), 7.31-7.45 (5H, m); MS m/e MH+ 281.

후처리

  1. customThe mixture was degassed 3 times
  2. temperaturethe mixture heated
  3. temperatureat reflux overnight
  4. temperatureThe reaction mixture was cooled
  5. extractionextracted with EtOAc (2×100 mL)
  6. washThe organic extracts were washed with water (100 mL)
  7. customdried
  8. customVolatile material was removed by evaporation and purification by chromatography

출처 및 근거

ORD 기록
ord-cfe364af517443f5b927cf917a5caa00
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07795283B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트