反应详情

温度

45 °C

Magnesium sulphate (9.6 g, 80 mmoles), DMA (2 g, 23 mmoles), (±)-3-methylpiperidine (4 g, 40 mmoles), tetrahydro-4H-thiopyran-4-one (2.3 g, 20 mmoles) and acetone cyanohydrin (1.7 g, 20 mmoles) are introduced in succession into a 250 ml two-necked flask. The reaction medium is agitated for 48 hours at 45° C. After cooling down to ambient temperature, the pasty mixture obtained is placed on ice (approximately 150) and agitated for 30 minutes. Extraction with ether is then carried out (3×80 ml), the combined organic phases are washed with water (100 ml), followed by drying over Na2SO4, filtering and concentration to dryness. A brown oil is thus obtained (4.5 g, 20 mmoles) constituted by a mixture of expected product with approximately 4% of amino nitrite originating from acetone and 7% of the remaining tetrahydro-4H-thiopyran-4-one. The product is then used without further purification.

1. temperatureAfter cooling down to ambient temperature
2. customthe pasty mixture obtained
3. stirringagitated for 30 minutes
4. extractionExtraction with ether
5. washthe combined organic phases are washed with water (100 ml)
6. dry with materialby drying over Na2SO4
7. filtrationfiltering
8. concentrationconcentration to dryness
9. customA brown oil is thus obtained (4.5 g, 20 mmoles)