2-Thiophenecarboxaldehyde → HCID 23369385、化合物
反応式
Cl.[NH2:2][CH2:3][CH2:4][C:5]([O:7][CH3:8])=[O:6].[S:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[CH:14]=O.[BH3-]C#N.[Na+]>CO>[S:9]1[CH:13]=[CH:12][CH:11]=[C:10]1[CH2:14][NH:2][CH2:3][CH2:4][C:5]([O:7][CH3:8])=[O:6]参加物
5
実験手順
To a stirring 25 mL MeOH solution of 1.40 g (10 mmol) of methyl β-alaninate hydrochloride and 1.34 g (12 mmol) of thiophene carboxaldehyde was added 1.26 g (20 mmol) of NaCNBH3. After 1 hour, 25 mL of saturated KHCO3 was added to the reaction. The reaction mixture was then filtered, and the resulting filtrate was extracted with 50 mL of DCM. The organic layer was treated as described above in Example 7, and the residue was chromatographed to yield 0.60 g (30%) of product. Analysis calculated for C9H13NO2S (M.W. 199.27): C, 54.25; H, 6.58; N, 7.03. Found: C, 54.02; H, 6.63; N, 6.77.
後処理
- filtrationThe reaction mixture was then filtered
- extractionthe resulting filtrate was extracted with 50 mL of DCM
- additionThe organic layer was treated
- customthe residue was chromatographed
出典と根拠
- ORDレコード
- ord-dbc2a81364eb42a3b22f4b10a787d43c
- 出典データセット
- uspto-grants-1995_11
- 特許番号
- US05464830
反応ノート
読み込み中…