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Ammonium formate → 6-Benzenesulfonyl-8-benzyl-1-phenyl-8-aza-bicyclo[3.2.1]octan-2-one

HRID 1244035
ノート
印刷プレビュー

反応式

HRID 1244035 の反応式
[C:1]1([S:7]([CH:10]2[CH2:16][C:15]3([C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)[N:17]([CH2:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:11]2[CH:12]=[CH:13][C:14]3=[O:31])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])=O.[NH4+]>[OH-].[Pd+2].[OH-].CO>[C:1]1([S:7]([CH:10]2[CH2:16][C:15]3([C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=4)[N:17]([CH2:18][C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=4)[CH:11]2[CH2:12][CH2:13][C:14]3=[O:31])(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 219318066-Benzenesulfonyl-8-benzyl-1-phenyl-8-aza-bicyclo[3.2.1]oct-3-en-2-one

生成物 1

HCID 219316456-Benzenesulfonyl-8-benzyl-1-phenyl-8-aza-bicyclo[3.2.1]octan-2-one

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 887Methanol溶媒

実験手順

To a 500 ml round bottom flask equipped with nitrogen inlet and condenser was placed 5.87 gm (13.68 mmol) of the 6-Benzenesulfonyl-8-benzyl-1-phenyl-8-aza-bicyclo[3.2.1]oct-3-en-2-one together with 150 ml of methanol, 17.25 gm (273.66 mmol) ammonium formate and 1.95 gm palladium hydroxide. The reaction mixture was heated under reflux for 1.5 hours and then cooled to room temperature. The suspension was filtered through a bed of celite which was then washed with methanol. The combined organics were evaporated in vacuo and the residue was taken up in chloroform and partitioned with saturated aqueous bicarbonate solution. The organics were washed with saturated brine solution and then dried over a bed of sodium sulfate. The mixture was filtered and the filtrate evaporated in vacuo. The residue was chromatographed on silica gel eluting with 8:2/hexane:ethyl acetate to afford 4.04 gm (68%) of an off white solid. 1H NMR (CDCl3, 400 MHz) δ 7.79 (d, 2H, J=7 Hz), 7.66 (t, 1H, J=7 Hz), 7.51 (t, 2H, J=8 Hz), 7.40–7.19 (m, 10H), 3.93 (br.s., 1H), 3.70 (d, 1H, J=15 Hz), 3.62 (t, 1H, J=7 Hz), 3.35 (d, 1H, J=14 Hz), 2.70–2.5 (m, 4H), 1.79–1.70 (m, 1H), 1.55 (br.s., 1H) ppm. Mass spectrum APCI m/z 432 (p+1).

後処理

  1. customTo a 500 ml round bottom flask equipped with nitrogen inlet and condenser
  2. temperatureThe reaction mixture was heated
  3. temperatureunder reflux for 1.5 hours
  4. filtrationThe suspension was filtered through a bed of celite which
  5. washwas then washed with methanol
  6. customThe combined organics were evaporated in vacuo
  7. custompartitioned with saturated aqueous bicarbonate solution
  8. washThe organics were washed with saturated brine solution
  9. dry with materialdried over a bed of sodium sulfate
  10. filtrationThe mixture was filtered
  11. customthe filtrate evaporated in vacuo
  12. customThe residue was chromatographed on silica gel eluting with 8:2/hexane
  13. customethyl acetate to afford 4.04 gm (68%) of an off white solid

出典と根拠

ORDレコード
ord-b2db8a3117224b92920270ec4bce00b4
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07119207B2

反応ノート

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