Trifluoroacetic acid → 3-Pyridylthio-2-phenylbenzoic acid

HRID 2121212노트

반응식

HRID 2121212 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 234363563-Pyridylthio-2-phenylbenzoic acid수율 101.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-3b720c296f1d4b178048e8ac1b95d411
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06693123B2

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