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

HRID 272602
ノート
印刷プレビュー

反応式

HRID 272602 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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%)

出典と根拠

ORDレコード
ord-de1932bdc7d549ae9694e0649e5f1e76
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07456177B2

反応ノート

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