Pyridine → 1-[(4-Nitrophenyl)sulfonyl]piperidine

HRID 1366823

反応式

HRID 1366823 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[N:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.N1CCCCC1>ClCCl>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

5

反応物 3

HCID 1049PyridineHCID 74044-Nitrobenzenesulfonyl chlorideHCID 8082Piperidine

生成物 1

HCID 7236241-[(4-Nitrophenyl)sulfonyl]piperidine収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 4-nitrobenzenesulfonyl chloride 40 g 0.181 mole in dichloromethane 400 ml was added over 30 mins a solution of pyridine 15 g 15.3 ml and piperidine 16.15 g 18.8 ml in dichloromethane 100 ml. The mixture was stirred at room temperature for 2 h and then washed with water, 2M hydrochloric acid and brine, dried MgSO4 and evaporated in vacuo to give 1-(4-nitro-benzenesulfonyl)-piperidine 44.5 g. 1HNMR CDCl3 7.76 (2H, d), 7.40 (2H, d), 3.21 (6H, q), 1.07 (6H, t).

後処理

  1. washwashed with water, 2M hydrochloric acid and brine, dried MgSO4
  2. customevaporated in vacuo

出典と根拠

ORDレコード
ord-a37ef5898cf1416d9d61c31bfd1f2d7b
出典データセット
uspto-grants-2011_02
特許番号
US07893077B2

関連ノート

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