Hydrochloric Acid → (E)-3-(6-aminopyrid-3-yl)acrylic acid hydrochloride
反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10]([O:12]C(C)(C)C)=[O:11])=[CH:4][CH:3]=1.FC(F)(F)C(O)=O.[ClH:24]>C(Cl)Cl.O1CCOCC1>[ClH:24].[NH2:1][C:2]1[N:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10]([OH:12])=[O:11])=[CH:4][CH:3]=1参加物
6
実験手順
To a solution of tert-butyl (2E)-3-(6-aminopyridin-3-yl)acrylate (380 mg, 1.73 mmol; which may be prepared as described in Step 1) in DCM (3.45 mL) under Argon was added trifluoroacetic acid (3.45 mL). The mixture was stirred at room temperature for 1 h, then HCl 4N in dioxane (6.9 mL) was added. A beige solid started precipitating at the half of the addition. After concentration, the solid was triturated in Et2O, filtered, rinsed with Et2O and dried under vacuum to give the title compound as a beige solid (265 mg, 76%).
後処理
- customA beige solid started precipitating at the half of the addition
- concentrationAfter concentration
- customthe solid was triturated in Et2O
- filtrationfiltered
- washrinsed with Et2O
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-01d563e223aa4f4db35a06d6fde3f07b
- 出典データセット
- uspto-grants-2015_06
- 特許番号
- US09051321B2
反応ノート
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