反应详情

A two-liter reaction flask with appropriate fittings was charged with 33.6 g (0.4 mole) of diketene, 965 ml of xylene and 59.7 g (0.38 mole) of 2-amino-5-tert butyl-1,3,4-thiadiazole. The stirred mixture was heated to 70° at which time all solids had dissolved. After one hour, the solution was cooled and added to 2500 ml of chilled heptane. Product precipitation was judged complete after two hours. The solids were collected on a vacuum filter and air dried. There was obtained 54 g (58.9%) of white product, m.p. 166°-68°. N.M.R. (CDCl3 -dimethyl-d6 sulfoxide) ∂ 1.5 [C(CH3)3 ], 2.0 (CH3, enol), 2.3 (CH3, keto), 3.6 (CH2), 5.4 (CH, enol).

1. customA two-liter reaction flask with appropriate fittings
2. temperatureThe stirred mixture was heated to 70° at which time all solids
3. dissolutionhad dissolved
4. temperaturethe solution was cooled
5. customProduct precipitation
6. waitwas judged complete after two hours
7. customThe solids were collected on a vacuum
8. filtrationfilter
9. customair dried