Methyl Thioglycolate → HCID 66934347、化合物

HRID 881553ノート

反応式

HRID 881553 の反応式
[H-].[Na+].[C:3]([O:7][CH3:8])(=[O:6])[CH2:4][SH:5].[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][CH:19](S(C)(=O)=O)[CH2:18][CH2:17]1)=[O:15])([CH3:12])([CH3:11])[CH3:10]>CN(C=O)C>[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][CH:19]([S:5][CH2:4][C:3]([O:7][CH3:8])=[O:6])[CH2:18][CH2:17]1)=[O:15])([CH3:12])([CH3:10])[CH3:11]

参加物

5

反応物 3

HCID 16907Methyl ThioglycolateHCID 24758Sodium hydrideHCID 22504298Tert-butyl 4-(methylsulfonyl)piperidine-1-carboxylate

生成物 1

HCID 66934347HCID 66934347、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To sodium hydride (60% wt. suspension in mineral oil, 108 mg) in dry DMF (5 ml) was added methyl thioglycolate (160 ul) dropwise at 0° C. After 30 minutes added 4-methanesulfonyl-piperidine-carboxylic acid tert-butyl ester (500 mg) as a solution in DMF (1.5 ml) and the reaction mixture was warmed up to room temperature over 5 hours. Aqueous work-up and purification on silica yielded 4-methoxycarbonylmethylsulfanyl-piperidine-1-carboxylic acid tert-butyl ester (414 mg).

後処理

  1. customAqueous work-up and purification on silica

出典と根拠

ORDレコード
ord-29a8218a8e7541918681ea23fdaa412d
出典データセット
uspto-grants-2015_03
特許番号
US08993563B2

反応ノート

読み込み中…