Sodium Hydroxide → 1-(3-chloropyridin-2-yl)-4-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]acetyl}-1H-pyrrole-2-carboxylic acid

HRID 874193ノート

反応式

HRID 874193 の反応式
[Cl:1][C:2]1[C:3]([N:8]2[CH:12]=[C:11]([C:13](=[O:24])[CH2:14][N:15]3[N:19]=[N:18][C:17]([C:20]([F:23])([F:22])[F:21])=[N:16]3)[CH:10]=[C:9]2[C:25]([O:27]C)=[O:26])=[N:4][CH:5]=[CH:6][CH:7]=1.[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[C:3]([N:8]2[CH:12]=[C:11]([C:13](=[O:24])[CH2:14][N:15]3[N:19]=[N:18][C:17]([C:20]([F:21])([F:22])[F:23])=[N:16]3)[CH:10]=[C:9]2[C:25]([OH:27])=[O:26])=[N:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 67125230methyl 1-(3-chloropyridin-2-yl)-4-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]acetyl}-1H-pyrrole-2-carboxylate

生成物 1

HCID 671252351-(3-chloropyridin-2-yl)-4-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]acetyl}-1H-pyrrole-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

130 mg (0.31 mmol) of methyl 1-(3-chloropyridin-2-yl)-4-{[5-(trifluoromethyl)-2H-tetrazol-2-yl]acetyl}-1H-pyrrole-2-carboxylate were dissolved in 3 ml of ethanol, 19 mg (0.47 mmol) of 2N aqueous sodium hydroxide solution were added and the mixture was stirred at RT for 4 h. The solvent was distilled off under reduced pressure, the residue was taken up in water and the mixture was extracted once with methyl tert-butyl ether. The aqueous phase was then acidified with 2N hydrochloric acid and extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulphate and concentrated.

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. extractionthe mixture was extracted once with methyl tert-butyl ether
  3. extractionextracted three times with ethyl acetate
  4. dry with materialThe combined organic phases were dried over sodium sulphate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-5c3d320cabb2457e890127bc1f6e0e3e
出典データセット
uspto-grants-2015_03
特許番号
US08980886B2

反応ノート

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