2-Thiophenecarboxaldehyde → HCID 23369385, 화합물
반응식
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]참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-dbc2a81364eb42a3b22f4b10a787d43c
- 출처 데이터셋
- uspto-grants-1995_11
- 특허 번호
- US05464830
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