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Thioglycolic Acid → HCID 178489398, 화합물

HRID 1865620
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HRID 1865620 반응식
C(OC([NH:8][C:9]1[CH:17]=[CH:16][C:15]([C:18]2[CH:19]=[C:20]3[C:26]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[O:33][CH3:34])=[N:25][N:24](COCC[Si](C)(C)C)[C:21]3=[N:22][CH:23]=2)=[CH:14][C:10]=1[C:11]([OH:13])=[O:12])=O)(C)(C)C.Cl(O)(=O)(=O)=O.SCC(O)=O>C(O)(=O)C.O>[NH2:8][C:9]1[CH:17]=[CH:16][C:15]([C:18]2[CH:19]=[C:20]3[C:26]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=4[O:33][CH3:34])=[N:25][NH:24][C:21]3=[N:22][CH:23]=2)=[CH:14][C:10]=1[C:11]([OH:13])=[O:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1133Thioglycolic AcidHCID 24247Perchloric AcidHCID 579759012-tert-butoxycarbonylamino-5-[3-(2-methoxy-phenyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-b]pyridin-5-yl]-benzoic acid

생성물 1

HCID 178489398HCID 178489398, 화합물수율 82.4%

시약·촉매·용매 2

HCID 176Acetic Acid용매
HCID 962
Water
용매
2회

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온도
80 °C

실험 절차

200 mg (0.34 mmol) of 2-tert-butoxycarbonylamino-5-[3-(2-methoxy-phenyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazolo[3,4-b]pyridin-5-yl]-benzoic acid were dissolved in 5 mL of glacial acetic acid. 500 μL of 70% perchloric acid was added and the mixture left at ambient temperature for 24 h. 3 mL of water and 300 μL of mercaptoacetic acid was added and the mixture heated to 80° C. for 20 h. The resulting mixture was cooled to room temperature and diluted with 50 mL of water. The resulting precipitate was filtered off and dried by suction to afford 101 mg (0.28 mmol, 82%) of 2-amino-5-[3-(2-methoxy-phenyl)-1H-pyrazolo[3,4-b]pyridin-5-yl]-benzoic acid as a red-brown solid. MS: m/z 361.1 (M+H+).

후처리

  1. temperatureThe resulting mixture was cooled to room temperature
  2. filtrationThe resulting precipitate was filtered off
  3. customdried by suction

출처 및 근거

ORD 기록
ord-33c0a24bbc004e02b41f2dbec3dfa8f8
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07626021B2

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