反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH3:29])[C:10]=1[C:11](=[O:28])[NH:12][C:13]1[CH:14]=[CH:15][C:16]2[N:17]([N:19]=[C:20]([N:22]3[CH2:27][CH2:26][O:25][CH2:24][CH2:23]3)[N:21]=2)[CH:18]=1)=[O:5])C.O.[OH-].[Li+]>CO.O>[CH3:29][N:9]1[C:10]([C:11](=[O:28])[NH:12][C:13]2[CH:14]=[CH:15][C:16]3[N:17]([N:19]=[C:20]([N:22]4[CH2:23][CH2:24][O:25][CH2:26][CH2:27]4)[N:21]=3)[CH:18]=2)=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]1参加物
5
反応物 2
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 55 °C
実験手順
A mixture of 1-methyl-5-(2-morpholin-4-yl-[1,2,4]triazolo[1,5-a]pyridin-6-ylcarbamoyl)-1H-pyrazole-4-carboxylic acid ethyl ester (282 mg, 0.71 mmol) and lithium hydroxide hydrate (88.9 mg, 2.12 mmol) in methanol (10 ml) and water (3 ml) was stirred for 18 hours at 55° C. The solvents were evaporated under reduced pressure and the residue treated with water (5 ml) and hydrogen chloride (1 molar in water, 2.12 ml). The precipitated solid was filtered off, washed with water and dried under reduced pressure, affording 1-methyl-5-(2-morpholin-4-yl-[1,2,4]triazolo[1,5-a]pyridin-6-ylcarbamoyl)-1H-pyrazole-4-carboxylic acid (187 mg, 71%) as light brown solid. Mp.: 294° C. MS: m/z=372.0 (M+H+).
後処理
- customThe solvents were evaporated under reduced pressure
- additionthe residue treated with water (5 ml) and hydrogen chloride (1 molar in water, 2.12 ml)
- filtrationThe precipitated solid was filtered off
- washwashed with water
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-fd719b818440472aad255ea0188e3d03
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09227970B2
関連ノート
読み込み中…