Sodium Hydroxide → Thieno[2,3-c]pyridine-5-carboxylic acid
反応式
[C:1]([CH:4]1[N:9](N=O)[CH2:8][C:7]2[S:12][CH:13]=[CH:14][C:6]=2[CH:5]1O)([OH:3])=[O:2].[OH-].[Na+]>C(O)C>[C:1]([C:4]1[CH:5]=[C:6]2[CH:14]=[CH:13][S:12][C:7]2=[CH:8][N:9]=1)([OH:3])=[O:2]参加物
4
実験手順
An initially homogeneous solution of 10 g (0.044 mole) of the nitroso derivative obtained in Example 1, 20 cc ethanol and 60 cc aqueous 20% sodium hydroxide is refluxed for 2 hours. After cooling and addition of ethanol, the resulting precipitate is filtered off, washed with ethanol and then with ether, after which it is dried. The resulting sodium salt (M.p.=260° C.; 4.7 g; 60%) is treated with 23 cc (1 equivalent) N hydrochloric acid. The material is found to dissolve at first and then to reprecipitate. It is directly recrystallized after addition of 27 cc water, to give 2.5 g (32%) pink crystals, M.p.=246° C.
後処理
- temperatureAfter cooling
- filtrationthe resulting precipitate is filtered off
- washwashed with ethanol
- dry with materialwith ether, after which it is dried
- additionThe resulting sodium salt (M.p.=260° C.; 4.7 g; 60%) is treated with 23 cc (1 equivalent) N hydrochloric acid
- dissolutionto dissolve at first and then
- customIt is directly recrystallized
- additionafter addition of 27 cc water
出典と根拠
- ORDレコード
- ord-90353734c9a5457b8426937635a2ea2c
- 出典データセット
- uspto-grants-1979_07
- 特許番号
- US04161599
反応ノート
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