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Water → methyl 1-(3-chloropyridin-2-yl)-3-{1-hydroxy-2-[5-(trifluoromethyl)-2H-tetrazol-2-yl]ethyl}-1H-pyrazole-5-carboxylate

HRID 1630675
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HRID 1630675 반응식
[H-].[Na+].[F:3][C:4]([F:11])([F:10])[C:5]1[N:6]=[N:7][NH:8][N:9]=1.[Cl:12][C:13]1[C:14]([N:19]2[C:23]([C:24]([O:26][CH3:27])=[O:25])=[CH:22][C:21]([CH:28]3[CH2:30][O:29]3)=[N:20]2)=[N:15][CH:16]=[CH:17][CH:18]=1.O>O1CCCC1.C(O)(=O)C>[Cl:12][C:13]1[C:14]([N:19]2[C:23]([C:24]([O:26][CH3:27])=[O:25])=[CH:22][C:21]([CH:28]([OH:29])[CH2:30][N:7]3[N:8]=[N:9][C:5]([C:4]([F:11])([F:10])[F:3])=[N:6]3)=[N:20]2)=[N:15][CH:16]=[CH:17][CH:18]=1
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참가 물질

7

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 4217082H-Tetrazole, 5-(trifluoromethyl)-, sodium salt (1:1)HCID 86661393methyl 1-(3-chloropyridin-2-yl)-3-(oxiran-2-yl)-1H-pyrazole-5-carboxylate

생성물 1

HCID 66587513methyl 1-(3-chloropyridin-2-yl)-3-{1-hydroxy-2-[5-(trifluoromethyl)-2H-tetrazol-2-yl]ethyl}-1H-pyrazole-5-carboxylate수율 80%

시약·촉매·용매

2
HCID 176Acetic Acid용매HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

51.5 mg (2.14 mmol) of sodium hydride were initially charged in 15 ml of tetrahydrofuran, and a solution of 1380 mg (2.32 mmol) of a 25% strength solution of 5-(trifluoromethyl)-2H-tetrazole in tetrahydrofuran was added at 0° C. After 20 minutes of stirring at 0° C., 500 mg (1.78 mmol) of methyl 1-(3-chloropyridin-2-yl)-3-(oxiran-2-yl)-1H-pyrazole-5-carboxylate were added, and the mixture was stirred at reflux temperature for 20 hours. The reaction mixture was poured into water, acidified with glacial acetic acid and then extracted repeatedly with ethyl acetate. The combined organic phases were washed with water and then dried over magnesium sulphate. The solvent was distilled off under reduced pressure and the residue was chromatographed on silica gel, which gave 286 mg (80% of theory) of methyl 1-(3-chloropyridin-2-yl)-3-{1-hydroxy-2-[5-(trifluoromethyl)-2H-tetrazol-2-yl]ethyl}-1H-pyrazole-5-carboxylate and methyl 1-(3-chloropyridin-2-yl)-3-{1-hydroxy-2-[5-(trifluoromethyl)-1H-tetrazol-1-yl]ethyl}-1H-pyrazole-5-carboxylate in a ratio of 66:34. (logP: 2.64/2.68; MH+: 418.0; 1H-NMR (400 MHz, CD3CN, δ, ppm): 3.73 (s, 3H), 4.31 (m, 2H), 4.48 (m, 1H), 7.10 (m, 1H), 7.54 (m, 1H), 8.05 (m, 1H), 8.50 (m, 1H).)

후처리

  1. stirringthe mixture was stirred
  2. temperatureat reflux temperature for 20 hours
  3. extractionextracted repeatedly with ethyl acetate
  4. washThe combined organic phases were washed with water
  5. dry with materialdried over magnesium sulphate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe residue was chromatographed on silica gel, which

출처 및 근거

ORD 기록
ord-8d464e599bd54244a4e09e49cc7d16cb
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08791139B2

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