Aluminium lithium hydride → Pyrazolo[1,5-a]pyridin-3-ylmethanol
反応式
C(=O)(O)N.[N:5]1[N:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]2=[C:7]([C:14](OC)=[O:15])[CH:6]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[N:5]1[N:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]2=[C:7]([CH2:14][OH:15])[CH:6]=1参加物
4
実験手順
A solution of methyl pyrazolo[1,5-a]pyridine-3-carboxylate carbamate (1) (400 mg, 2.10 mmol) in THF (4 mL) was added LiAlH4 (159 mg, 4.20 mmol) at room temperature for 1 h. The reaction mixture was concentrated and 10 mL sat. aq. NaHCO3 was added, extracted with EA (3×10 mL). The organic phase was dried with anhydrous Na2SO4, filtered and concentrated. The residue was purified by Prep-TLC TLC using PE/EtOAc=2/1 to give title compound as oil.
後処理
- concentrationThe reaction mixture was concentrated
- addition10 mL sat. aq. NaHCO3 was added
- extractionextracted with EA (3×10 mL)
- dry with materialThe organic phase was dried with anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by Prep-TLC TLC
出典と根拠
- ORDレコード
- ord-616d62769ecc4722abec24a2b02f8f51
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09353104B2
反応ノート
読み込み中…