反応式
[NH2:1][C:2]1[S:3][C:4]2[CH:10]=[C:9]([O:11][C:12]([F:15])([F:14])[F:13])[CH:8]=[CH:7][C:5]=2[N:6]=1.Cl[CH2:17][CH2:18][NH:19][C:20](=[O:22])[CH3:21].[I-].[Na+]>C(C(C)=O)C>[C:20]([NH:19][CH2:18][CH2:17][N:6]1[C:5]2[CH:7]=[CH:8][C:9]([O:11][C:12]([F:15])([F:13])[F:14])=[CH:10][C:4]=2[S:3][C:2]1=[NH:1])(=[O:22])[CH3:21]参加物
反応条件
- 温度
- 20 °C
実験手順
2-Amino-6-trifluoromethoxybenzothiazole (9.4 g), N(2-chloroethyl)acetamide (9.7 g) and sodium iodide (13.5 g) in methyl ethyl ketone (30 cc) are heated for 40 hours to boiling. After cooling to a temperature in the region of 20° C., the reaction medium is added to distilled water (200 cc), treated with IN sodium hydroxide (40 cc) and then extracted with ethyl acetate (200 cc). After drying over magnesium sulphate and then concentration to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa), the residue is purified by chromatography on a silica column with a mixture of ethyl acetate and methanol (90:10 by volume) as eluent. 3-(2-Acetamidoethyl)-2-imino-6-trifluoromethoxybenzothiazoline (2.7 g) is obtained, which product is converted to a hydrochloride subliming at about 180° C.
後処理
- additionthe reaction medium is added
- distillationto distilled water (200 cc)
- additiontreated with IN sodium hydroxide (40 cc)
- extractionextracted with ethyl acetate (200 cc)
- dry with materialAfter drying over magnesium sulphate
- concentrationconcentration to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa)
- customthe residue is purified by chromatography on a silica column with a mixture of ethyl acetate and methanol (90:10 by volume) as eluent
出典と根拠
- ORDレコード
- ord-834f28866e1046d99f9122dd971a08ff
- 出典データセット
- uspto-grants-1991_06
- 特許番号
- US05026717
関連ノート
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