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Methyl iodide → 6-chloro-3-methoxy-4-methyl-1-trityl-1H-pyrazolo[4,3-c]pyridine

HRID 588087
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HRID 588087 반응식
[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]2[C:9](=[O:31])[NH:10][N:11]([C:12]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:4]=2[CH:3]=1.[C:32](=O)([O-])[O-].[K+].[K+].CI>CN(C=O)C.O>[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]2[C:9]([O:31][CH3:32])=[N:10][N:11]([C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)[C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:4]=2[CH:3]=1
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참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 1182721366-chloro-4-methyl-1-trityl-1H-pyrazolo[4,3-c]pyridin-3(2H)-one2회

생성물 1

HCID 1182721496-chloro-3-methoxy-4-methyl-1-trityl-1H-pyrazolo[4,3-c]pyridine

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

실험 절차

A solution of 6-chloro-4-methyl-1-trityl-1H-pyrazolo[4,3-c]pyridin-3(2H)-one (Intermediate 4B; 406 mg, 0.953 mmol) in DMF (3 mL) was charged with potassium carbonate (348 mg, 2.52 mmol) and methyl iodide (0.089 mL, 1.430 mmol) and stirred at room temperature for 1 h. The reaction mixture was diluted with water, filtered, and dried under vacuum to give 6-chloro-3-methoxy-4-methyl-1-trityl-1H-pyrazolo[4,3-c]pyridine, which was carried onto the next step without further purification. MS ESI calc'd. for C27H22ClN3O [M+1]+ 440. found 440.

후처리

  1. filtrationfiltered
  2. customdried under vacuum

출처 및 근거

ORD 기록
ord-d78f7bdde08e4323bfbaa895c16dc85f
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09226922B2

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