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Benzylamine → 11-(Phenylmethyl)-3,11-diazatricyclo[7.3.1.02,7]trideca-2,4,6-triene

HRID 1727183
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HRID 1727183 반응식
[CH:1]12[CH2:14][CH:9]([CH:10](O)[CH:11]1O)[CH2:8][C:7]1[C:2]2=[N:3][CH:4]=[CH:5][CH:6]=1.I([O-])(=O)(=O)=O.[Na+].[CH2:21]([NH2:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>C(O)C.O.ClC(Cl)C.C(OCC)(=O)C>[C:22]1([CH2:21][N:28]2[CH2:11][CH:1]3[CH2:14][CH:9]([CH2:8][C:7]4[C:2]3=[N:3][CH:4]=[CH:5][CH:6]=4)[CH2:10]2)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
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참가 물질

10

반응물 5

HCID 7504BenzylamineHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 23667635Sodium periodateHCID 688083706,7,8,9-Tetrahydro-5H-6,9-methanocyclohepta[b]pyridine-7,8-diol

생성물 1

HCID 5983784111-(Phenylmethyl)-3,11-diazatricyclo[7.3.1.02,7]trideca-2,4,6-triene
수율 50%

시약·촉매·용매 4

HCID 702Ethanol용매HCID 962Water용매2회HCID 63651,1-Dichloroethane용매HCID 8857Ethyl Acetate용매2회

실험 절차

To a solution of 3-azatricyclo[7.2.1.02,7]dodeca-2,4,6-triene-10,11-diol (Preparation 24, 1.16 g, 6.07 mmol) in ethanol (40 ml) was added sodium periodate (1.35 g, 6.07 mmol) in water (20 ml) to produce a yellow slurry. After 15 min, water and ethyl acetate were added and the layers were separated, the aqueous layer washed with ethyl acetate (4×50 ml) and then dichloromethane. The combined organic extracts were dried (Na2SO4) to give an orange oil. The oil was diluted with dichloroethane (50 ml), benzylamine (0.65 g, 6.07 mmol) was added followed by sodium triacetoxyborohydride (4.12 g, 19.4 mmol). After 7 h, saturated sodium hydrogen carbonate solution (75 ml) and ethyl acetate (75 ml) were added and the reaction mixture was stirred for 20 min. The layers were separated and the aqueous layer was extracted with ethyl acetate (2×50 ml). The combined organic extracts were washed with water and brine, and then dried (Na2SO4) and concentrated in vacuo to give the crude product. Purification by flash chromatography produced the title compound as a light yellow oil (0.80 g, 50%).

후처리

  1. customto produce a yellow slurry
  2. customthe layers were separated
  3. washthe aqueous layer washed with ethyl acetate (4×50 ml)
  4. dry with materialThe combined organic extracts were dried (Na2SO4)
  5. customto give an orange oil
  6. additionwas added
  7. waitAfter 7 h
  8. customThe layers were separated
  9. extractionthe aqueous layer was extracted with ethyl acetate (2×50 ml)
  10. washThe combined organic extracts were washed with water and brine
  11. dry with materialdried (Na2SO4)
  12. concentrationconcentrated in vacuo
  13. customto give the crude product
  14. customPurification by flash chromatography

출처 및 근거

ORD 기록
ord-86e926c912d34b0bae22a3115bbc3bf3
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07494992B2

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