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Ammonium Hydroxide → 11-(2-Benzyl-2,5-diazabicyclo(2.2.1) hept-5-yl)-dibenz[b,f][1,4]oxazepine

HRID 1457533
ノート
印刷プレビュー

反応式

HRID 1457533 の反応式
O=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[NH:3]1.[CH2:17]([N:24]1[CH2:29][C@@H:28]2[CH2:30][C@H:25]1[CH2:26][NH:27]2)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[NH4+].[OH-]>C1(C)C=CC=CC=1.Cl[Ti](Cl)(Cl)Cl>[CH2:17]([N:24]1[CH2:29][CH:28]2[CH2:30][CH:25]1[CH2:26][N:27]2[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[O:6][C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[N:3]=1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][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

6

反応物 3

HCID 14923Ammonium HydroxideHCID 72374O-(o-Aminophenoxy)benzoic acid lactamHCID 14612543(1S,4S)-2-Benzyl-2,5-Diazabicyclo[2.2.1]heptane

生成物 1

HCID 2209953111-(2-Benzyl-2,5-diazabicyclo(2.2.1) hept-5-yl)-dibenz[b,f][1,4]oxazepine

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒
HCID 1140
Toluene
溶媒

実験手順

To a solution of 11-oxo-dibenz[b,f][1,4]oxazepine (Aldrich) (0.149 g, 0.0007 mol) in dry toluene (10 mL), was added (1S,4S)-2-benzyl-2,5-diazabicyclo(2.2.1)heptane (0.54 g, 0.003 mol) and TiCl4 (0.75 mL, 0.0008 mol) via syringe. The mixture was stirred at room temperature for 30 min then refluxed for 5 hrs. The reaction mixture was cooled and dumped into conc. NH4OH and extracted with CHCl3. The combined organic phases were dried (MgSO4) and concentrated in vacuo. The crude material was chromatographed (hexane:EtOAc, 1:1) to give 11-(2-benzyl-2,5-diazabicyclo(2.2.1) hept-5-yl)-dibenz[b,f][1,4]oxazepine (yield 0.1319, mp 70°-72° C.).

後処理

  1. temperaturethen refluxed for 5 hrs
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with CHCl3
  4. dry with materialThe combined organic phases were dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe crude material was chromatographed (hexane:EtOAc, 1:1)

出典と根拠

ORDレコード
ord-97bf18cabca54857a42dcc76a5bafa99
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05849734

反応ノート

読み込み中…

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