تفاعل #1869147
ord-817cd11527084050ab0e75f85e5e8e0a
معادلة التفاعل
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المعالجة
- 1درجة الحرارةTo the solution cooled
- 2أخرىexceed 10° C
- 3أخرىThe organic layer was separated
- 4غسيلwashed with 150 g of water three times
- 5تركيزThe organic layer was concentrated in vacuum
- 6workup.ADDITIONMethanol was added to the
- 7تركيزconcentrate for recrystallization
- 8ترشيحfollowed by filtration
- 9أخرىdrying
- 10أخرىThere were obtained crude yellow crystals
- 11أخرىThe crude yellow crystals were purified by silica gel column chromatography (eluent, dichloromethane)
- 12تركيزThe elute was concentrated
- 13أخرىfollowed by recrystallization from methanol, filtration
- 14أخرىdrying
الإجراء التجريبي
In 490 g of tetrahydrofuran were dissolved 45 g (0.19 mol) of (3-(hydroxy)imino-3H-thiophen-2-ylidene)-(2-methylphenyl)-acetonitrile in Synthesis Example 1 and 27.0 g (0.19 mol) of commercially available propanesulfonyl chloride. To the solution cooled, 20.6 g (0.20 mol) of triethylamine was added dropwise such that the temperature might not exceed 10° C. The solution was allowed to ripen for 1 hour at room temperature, after which 150 g of water and 500 g of dichloromethane were added. The organic layer was separated, and washed with 150 g of water three times. The organic layer was concentrated in vacuum. Methanol was added to the concentrate for recrystallization, followed by filtration and drying. There were obtained crude yellow crystals. The crude yellow crystals were purified by silica gel column chromatography (eluent, dichloromethane). The elute was concentrated, followed by recrystallization from methanol, filtration and drying. There was obtained 77 g of yellow crystals (yield 70%).