Sodium Hydroxide → 3,5-Dichloro-4-methoxyaniline
반응식
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[C:4]([Cl:11])[C:3]=1[O:12][CH3:13].O.O.[Sn](Cl)Cl.[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([CH:5]=[C:4]([Cl:11])[C:3]=1[O:12][CH3:13])[NH2:8]참가 물질
5
실험 절차
A stirred mixture of 2,6-dichloro-4-nitroanisole (4.6 g, 21 mM) and tin(II) dichloride dihydrate (23.4 g, 104 mM) in ethanol (72 mL) was refluxed for 3 hr. After cooling to room temperature, the reaction mixture was poured into ice water which was then treated with 2N sodium hydroxide until the solution became basic. The resulting mixture was filtered through diatomaceous earth and the filtrate was extracted with ethyl acetate. The combined ethyl acetate extracts were dried (MgSO4), filtered and concentrated to obtain (3.33 g, 83.7%) the title compound as a yellow-brown solid, mp 80°-81° C.; MS(CI): 192 (M+H).
후처리
- temperaturewas refluxed for 3 hr
- filtrationThe resulting mixture was filtered through diatomaceous earth
- extractionthe filtrate was extracted with ethyl acetate
- dry with materialThe combined ethyl acetate extracts were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-d1949a80f5a34ab9a1a505ee7b40c299
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05733910
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