Water → 5-Cyano-2,3-dihydro-3,3-dimethyl-2-isothiocyanatobenzofuran
反応式
Cl[CH:2]1[C:6]([CH3:8])([CH3:7])[C:5]2[CH:9]=[C:10]([C:13]#[N:14])[CH:11]=[CH:12][C:4]=2[O:3]1.[S-:15][C:16]#[N:17].[K+].O>CN(C)C=O>[C:13]([C:10]1[CH:11]=[CH:12][C:4]2[O:3][CH:2]([N:17]=[C:16]=[S:15])[C:6]([CH3:8])([CH3:7])[C:5]=2[CH:9]=1)#[N:14]参加物
5
実験手順
2-Chloro-5-cyano-2,3-dihydro-3,3-dimethylbenzofuran (5 g) from Example 15 and potassium thiocyanate (4.6 g) were heated in dimethylformamide (30 ml) at 110° C. for 7 hours. The mixture, after cooling, was added to water and the product extracted into diethyl ether. The ether solution was washed with water (twice), dried over magnesium sulphate and run down under vacuum yielding 4 g of crude product. Purification by silica gel chromatography in toluene yielded 1.2 g of title product, mp 52° C.
後処理
- temperatureThe mixture, after cooling
- extractionthe product extracted into diethyl ether
- washThe ether solution was washed with water (twice),
- dry with materialdried over magnesium sulphate
- customyielding 4 g of crude product
- customPurification by silica gel chromatography in toluene
出典と根拠
- ORDレコード
- ord-632947a72b384ee4833bda6bef6d884f
- 出典データセット
- uspto-grants-1981_04
- 特許番号
- US04263037
反応ノート
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