Sodium Hydroxide → 4,5,6,7-Tetrahydro-1H-indazole-3-carboxylic acid
反応式
C([O:3][C:4]([C:6]1[C:14]2[CH2:13][CH2:12][CH2:11][CH2:10][C:9]=2[NH:8][N:7]=1)=[O:5])C.[OH-].[Na+]>CO>[NH:8]1[C:9]2[CH2:10][CH2:11][CH2:12][CH2:13][C:14]=2[C:6]([C:4]([OH:5])=[O:3])=[N:7]1参加物
4
実験手順
A solution of 4,5,6,7-tetrahydro-1H-indazole-3-carboxylic acid ethyl ester [0.606 g, Reference Example 18(a)] in methanol (50 ml) was treated with sodium hydroxide (0.500 g). The mixture was refluxed for 16 hours, then cooled and then evaporated. The residual white solid was treated with hydrochloric acid (30 ml, 2N) and the resulting solution was extracted three times with ethyl acetate (50 ml). The combined organic extracts were dried over sodium sulfate and then evaporated to yield 4,5,6,7-tetrahydro-1H-indazole-3-carboxylic acid (0.424 g) as a white solid. LC-MS (METHOD B): RT=2.44 minutes; 167 (M+H)+.
後処理
- temperatureThe mixture was refluxed for 16 hours
- temperaturecooled
- customevaporated
- additionThe residual white solid was treated with hydrochloric acid (30 ml, 2N)
- extractionthe resulting solution was extracted three times with ethyl acetate (50 ml)
- dry with materialThe combined organic extracts were dried over sodium sulfate
- customevaporated
出典と根拠
- ORDレコード
- ord-b50ccbe39e3a45fdb4929b6ff99e8427
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08288425B2
反応ノート
読み込み中…