Trifluoroacetic acid → Piperidine-4-carbothioic acid S-phenyl ester

HRID 713457

反応式

HRID 713457 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([S:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[C:17]1([S:16][C:14]([CH:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)=[O:15])[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 893758004-Phenylsulfanylcarbonyl-piperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 89389269Piperidine-4-carbothioic acid S-phenyl ester収率 98.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-phenylsulfanylcarbonyl-piperidine-1-carboxylic acid tert-butyl ester (1.11 g, 3.45 mmol) in 10 mL of DCM, was added 2 mL of TFA. The reaction mixture was stirred at ambient temperature for 2.5 hours then solvent was removed by reduced pressure to yield the title product (0.75 g, 3.4 mmol). MS (ESI) m/z 221.8 (M+H+); HPLC (Novapak 150×3.9 mm C-18 column: mobile phase: 35-90% acetonitrile/water with 0.1% TFA, at 2 mL/min over 2 min.) t 1.29 min.

後処理

  1. customsolvent was removed by reduced pressure

出典と根拠

ORDレコード
ord-45688cec6cf04e49adae31a0068a814a
出典データセット
uspto-grants-2015_11
特許番号
US09181266B2

関連ノート

読み込み中…