反应详情

In procedures as noted in Example 1, a reaction mixture of 4-hydrazino-2,3,5-trichloro-6-(trichloromethyl)pyridine (9.9 grams; 0.03 mole) and sodium hydroxide (1/N, 37.5 ml, 0.0375 mole) in methanol (100 ml) was heated under reflux conditions for a period of about 4 hours and the product similarly recovered as a brown oil. Examination of GLC, PMR and mass spectral analysis indicated a product yield of 59% of 3,5,6-trichloro-2-(dichloromethyl)pyridine. A portion of the crude product was distilled over at 168°-73° C./21 mmHg as a colorless oil which crystallized as large colorless prisms from hexane, m.p. 61°-62° C.

1. temperaturewas heated under reflux conditions for a period of about 4 hours
2. customthe product similarly recovered as a brown oil