ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

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

HRID 1630675
ノート
印刷プレビュー

反応式

HRID 1630675 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒

2
HCID 176Acetic Acid溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

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).)

後処理

  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

出典と根拠

ORDレコード
ord-8d464e599bd54244a4e09e49cc7d16cb
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08791139B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート