Pyridine, 3-chloro-, 1-oxide → 3-Piperidin-1-ylpyridine 1-oxide

HRID 251058

反応式

HRID 251058 の反応式
Cl[C:2]1[CH:3]=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=1>N1CCCCC1>[N:4]1([C:2]2[CH:3]=[N+:4]([O-:8])[CH:5]=[CH:6][CH:7]=2)[CH2:5][CH2:6][CH2:7][CH2:2][CH2:3]1

参加物

3

反応物 1

HCID 123133Pyridine, 3-chloro-, 1-oxide

生成物 1

HCID 8174083-Piperidin-1-ylpyridine 1-oxide収率 133.4%

試薬・触媒・溶媒 1

HCID 8082Piperidine溶媒

実験手順

A solution of 3-chloro-pyridine 1-oxide (2.40 g, 18.5 mmol) in piperidine (6 mL) was heated at 140° C. for 2 days. After the reaction mixture was cooled to room temperature the amine was removed, and the residue was purified by flash chromatography on a silica gel column (6:1 EtOAc/MeOH), affording 3,4,5,6-tetrahydro-2H-[1,3′]bipyridinyl 1′-oxide as a pale yellow solid (2.20 g, 67%). 1H NMR (CDCl3) δ 1.59-1.67 (m, 6H), 3.14-3.18 (m, 4H), 6.78 (dd, 1H, J=2.1, 8.7 Hz), 7.03 (dd, 1H, J=6.3, 8.7 Hz), 7.63-7.66 (m, 1H), 7.85-7.86 (m, 1H).

後処理

  1. customwas removed
  2. customthe residue was purified by flash chromatography on a silica gel column (6:1 EtOAc/MeOH)

出典と根拠

ORDレコード
ord-d733a3b63baf4b3a882717a762111948
出典データセット
uspto-grants-2011_01
特許番号
US07863293B2

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