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8-Benzyl-3-(tert-butoxycarbonyl)-3,8-diazabicyclo[3.2.1]octane hydrochloride → tert-Butyl 3,8-diazabicyclo[3.2.1]octane-3-carboxylate hydrochloride

HRID 1743697
ノート
印刷プレビュー

反応式

HRID 1743697 の反応式
[ClH:1].C([N:9]1[CH:14]2[CH2:15][CH2:16][CH:10]1[CH2:11][N:12]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:13]2)C1C=CC=CC=1.[H][H]>[Pd].CO>[ClH:1].[CH:10]12[NH:9][CH:14]([CH2:15][CH2:16]1)[CH2:13][N:12]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:11]2
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 222354058-Benzyl-3-(tert-butoxycarbonyl)-3,8-diazabicyclo[3.2.1]octane hydrochlorideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 22235404tert-Butyl 3,8-diazabicyclo[3.2.1]octane-3-carboxylate hydrochloride収率 97.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

Palladium on carbon (10% w/w, 500 mg) was added to a solution of 8-benzyl-3-(tert-butoxycarbonyl)-3,8-diazabicyclo[3.2.1]octane hydrochloride (16.5 g, 48.0 mmol, see step (h) above) in methanol (250 mL) under a nitrogen atmosphere at 25° C. The nitrogen atmosphere was exchanged for a hydrogen atmosphere (1 atm of pressure) and the reaction was stirred rapidly. After 4 h the stirring was stopped and the reaction was filtered through a pad of Celite®. The filtrate was concentrated in vacuo to afford an off-white solid (11.6 g). The solid was slurried in acetonitrile, collected and dried in vacuo to afford 10.5 g (86%) of the title compound.

後処理

  1. filtrationthe reaction was filtered through a pad of Celite®
  2. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-d3f10bab6df0452b985e0b20e8895027
出典データセット
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07012074B2

反応ノート

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