Hydrochloric Acid → HCID 86674697、化合物
反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([CH2:13][CH3:14])[N:12]=1)[C:6]([O:8]C)=[O:7])#[N:2].[Li+].[OH-].Cl>C1COCC1.CO.O>[CH2:13]([C:11]1[CH:10]=[C:5]([C:6]([OH:8])=[O:7])[CH:4]=[C:3]([C:1]#[N:2])[N:12]=1)[CH3:14]参加物
7
反応条件
- 温度
- 2.5 °C
実験手順
Under N2, methyl 2-cyano-6-ethylisonicotinate (0.233 g, 1.23 mmol, Eq: 1.00) was diluted in THF (12.1 ml) and MeOH (1.46 ml). At 2-3° C., 1M LiOH in water (1.53 ml, 1.53 mmol, Eq: 1.25) was added dropwise (over 3 min) The RM was stirred at 2-3° C. for 30 minutes. Control with TLC: the reaction was finished. The reaction mixture was acidified with 1M HCl. The mixture was diluted with H2O and extracted with EtOAc. The organic phase was dried over MgSO4; filtered; concentrated in vacuo. White solid. MS (EIC): 174.9 ([M−H]−)
後処理
- extractionextracted with EtOAc
- dry with materialThe organic phase was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-3096321411864631b6b917d9982e9a15
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09029370B2
反応ノート
読み込み中…