tert-Butyl (pyridin-3-ylmethyl)carbamate → tert-butyl N-[(piperidin-3-yl)methyl]carbamate

HRID 16246ノート

反応式

HRID 16246 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH:2]=1>C(O)C.[Rh]>[NH:1]1[CH2:6][CH2:5][CH2:4][CH:3]([CH2:7][NH:8][C:9](=[O:15])[O:10][C:11]([CH3:13])([CH3:12])[CH3:14])[CH2:2]1

参加物

4

反応物 1

HCID 13948280tert-Butyl (pyridin-3-ylmethyl)carbamate

生成物 1

HCID 2756030tert-butyl N-[(piperidin-3-yl)methyl]carbamate

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒HCID 702Ethanol溶媒

実験手順

A mixture of tert-butyl 3-pyridinylmethylcarbamate (4.3 g) and 5% rhodium on carbon (400 mg) in ethanol (50 mL) at 25° C. in a paar apparatus was stirred under hydrogen at 60 pounds per square inch for 27 hours, filtered through diatomaceous earth (Celite®), and concentrated. 1H NMR (300 MHz, CDCl3) δ 4.55 (b, 1H), 2.99 (m, 4H), 2.56 (t, 1H), 2.33 (t, 1H), 1.74 (m, 1H), 1.66 (m, 2H), 1.44 (s, 9H).

後処理

  1. filtrationfiltered through diatomaceous earth (Celite®)
  2. concentrationconcentrated

出典と根拠

ORDレコード
ord-768044a1ab7e49fcbb115dd49f558187
出典データセット
uspto-grants-2010_06
特許番号
US07737159B2

反応ノート

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