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

Acetic Acid → 11-Allyl-6-methoxy-11-aza-tricyclo[7.3.1.02,7]trideca-2(7),3,5-trien-8-one

HRID 272602
노트
인쇄 미리보기

반응식

HRID 272602 반응식
O[CH:2]1[CH:8](O)[CH:7]2[CH2:10][CH:3]1[C:4]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[C:5]=1[C:6]2=[O:11].[C:18]([O-])(=O)[CH3:19].C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.[Pb+4].CC(O)=O.[CH2:39]([NH2:42])C=C.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C([O-])([O-])=O.[Na+].[Na+]>ClCCl>[CH2:39]([N:42]1[CH2:2][CH:3]2[CH2:10][CH:7]([C:6](=[O:11])[C:5]3[C:12]([O:16][CH3:17])=[CH:13][CH:14]=[CH:15][C:4]=32)[CH2:8]1)[CH:18]=[CH2:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 176Acetic AcidHCID 7853AllylamineHCID 10340Sodium CarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 598378516,7-Dihydroxy-1-methoxy-5,6,7,8-tetrahydro-5,8-methano-benzocyclohepten-9-oneHCID 178418268HCID 178418268, 화합물

생성물 1

HCID 59837863
11-Allyl-6-methoxy-11-aza-tricyclo[7.3.1.02,7]trideca-2(7),3,5-trien-8-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

6,7-Dihydroxy-1-methoxy-5,6,7,8-tetrahydro-5,8-methano-benzocyclohepten-9-one (2.80 g, 12 mmol) was stirred at 0° C. in dichloromethane (15 mL) and treated with lead tetraacetate (Pb(OAc)4, 5.35 g, 12 mmol). After 30 min. the mixture was filtered through a Celite™ pad and rinsed with dichloromethane (50 mL). To the stirred filtrate was added AcOH (3.61 g, 60 mmol) and allyl amine (689 mg, 12 mmol). After 15 min., the mixture was treated with NaBH(OAc)3 (7.70 g, 36 mmol) and stirred for 18 h. The mixture was poured into a saturated aqueous Na2CO3 solution (100 mL) stirred for 30 min. The layers were separated and extracted with EtOAc (2×100 mL). The organic layer was washed with a saturated aqueous Na2CO3 solution (2×50 mL), H2O (50 mL), saturated aqueous NaCl solution (50 mL), dried over MgSO4, filtered and concentrated to an oil. Purification by chromatography on silica gel eluting with 5% EtOAc/hexanes provided product as an oil (885 mg, 29%). (TLC 30% EtOAc/hexanes Rf 0.67).

후처리

  1. filtrationAfter 30 min. the mixture was filtered through a Celite™ pad
  2. washrinsed with dichloromethane (50 mL)
  3. stirringstirred for 30 min
  4. customThe layers were separated
  5. extractionextracted with EtOAc (2×100 mL)
  6. washThe organic layer was washed with a saturated aqueous Na2CO3 solution (2×50 mL), H2O (50 mL), saturated aqueous NaCl solution (50 mL)
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated to an oil
  10. customPurification by chromatography on silica gel eluting with 5% EtOAc/hexanes provided product as an oil (885 mg, 29%)

출처 및 근거

ORD 기록
ord-de1932bdc7d549ae9694e0649e5f1e76
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07456177B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트