反应详情

140 g of the product of Example 1 and 210 ml of demineralized water are introduced at 20°±2° C., agitation is carried out and 210 ml of pure 22°Be hydrochloric acid is added over about 5 minutes. The reaction medium is maintained at 35°-40° C. for 30 minutes under agitation then cooled down to 0°±5° C. under agitation. Then 28 ml of methylene chloride is added, a solution of 43.7 g of sodium nitrite in 70 ml of demineralized water is then added over about 30 minutes, at 0°±5° C. The reaction medium is maintained for another hour under agitation at 0°±5° C., a solution of 87.7 g of sodium iodide in 140 ml of demineralized water is added over 45 minutes. The reaction medium is maintained under agitation for another hour and 700 ml of methylene chloride is added. Agitation is carried out for 15 minutes at 0°±5° C., 28 g of sodium metabisulphite is added in one go and agitation is carried out for another 30 minutes while leaving the temperature to return to 20° C. After pouring, the organic phase is decanted, the aqueous phase is reextracted with 280 ml of methylene chloride, then the organic phases are washed with 3×140 ml of a saturated aqueous solution of NaCl. The joint chloromethylenic phases are dried, followed by filtering and washing with 3×70 ml of methylene chloride and 184.5 g of expected product (white crystals) is obtained, M.p.=164-165° C.

1. temperatureThe reaction medium is maintained at 35°-40° C. for 30 minutes under agitation
2. temperaturethen cooled down to 0°±5° C. under agitation
3. temperatureThe reaction medium is maintained for another hour under agitation at 0°±5° C.
4. temperatureThe reaction medium is maintained under agitation for another hour
5. waitis carried out for another 30 minutes
6. customwhile leaving the temperature
7. customto return to 20° C
8. additionAfter pouring
9. customthe organic phase is decanted
10. washthe organic phases are washed with 3×140 ml of a saturated aqueous solution of NaCl
11. customThe joint chloromethylenic phases are dried
12. filtrationby filtering
13. washwashing with 3×70 ml of methylene chloride