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

HRID 1727183
ノート
印刷プレビュー

反応式

HRID 1727183 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 702Ethanol溶媒HCID 962Water溶媒2 回HCID 63651,1-Dichloroethane溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-86e926c912d34b0bae22a3115bbc3bf3
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07494992B2

反応ノート

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