Trifluoroacetic acid → 3-Pyridylthio-2-phenylbenzoic acid

HRID 2121212ノート

反応式

HRID 2121212 の反応式
C([O:5][C:6](=[O:26])[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([S:13][C:14]2[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=2)[C:8]=1[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)(C)(C)C.C([SiH](CC)CC)C.FC(F)(F)C(O)=O>ClCCl>[N:16]1[CH:17]=[CH:18][CH:19]=[C:14]([S:13][C:9]2[C:8]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[C:7]([CH:12]=[CH:11][CH:10]=2)[C:6]([OH:26])=[O:5])[CH:15]=1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 538048533-Pyridylthio-2-phenylbenzoic acid tert-butyl ester

生成物 1

HCID 234363563-Pyridylthio-2-phenylbenzoic acid収率 101.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a 0° C. solution in dichloromethane (1 mL) of 3-pyridylthio-2-phenylbenzoic acid tert-butyl ester (245 mg, 0.67 mmol), prepared as in Example 241 A, and triethylsilane (390 mg, 3.4 mmol) was added trifluoroacetic acid (1.53 g, 13.4 mmol) and the reaction mixture was warmed to ambient temperature and stirred for 18 hours. The reaction mixture was concentrated and azeotroped with toluene (3×) to give 3-pyridylthio-2-phenylbenzoic acid (209 mg) as a translucent film which was used without further purification.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customazeotroped with toluene (3×)

出典と根拠

ORDレコード
ord-3b720c296f1d4b178048e8ac1b95d411
出典データセット
uspto-grants-2004_02
特許番号
US06693123B2

反応ノート

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