Sodium Hydroxide → 3,5-Dichloro-4-methoxyaniline
反応式
[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]参加物
5
実験手順
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 liltrate 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).
後処理
- temperaturewas refluxed for 3 hr
- filtrationThe resulting mixture was filtered through diatomaceous earth
- extractionthe liltrate was extracted with ethyl acetate
- dry with materialThe combined ethyl acetate extracts were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-9f58e1ca23af46649bde517da2437f91
- 出典データセット
- uspto-grants-1997_02
- 特許番号
- US05599814
反応ノート
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