反应详情

18 Grams of sodium chloride were added in about 20 equal portions to a mixture of 3 g of 1-adamantyl-acetic acid, 60 ml. of carbon tetrachloride and 200 g of 96% sulfuric acid which was kept at 5° -10°C by external cooling under thorough stirring over a period of 6 hours while a mixture of 9 g of t-butanol and 20 ml. of carbon tetrachloride was added thereto dropwise over 30 minutes. The reaction mixture was poured onto 300 g of broken ice pieces. The crystalline precipitate was filtered out, washed with water sufficiently and air-dried to obtain 3.2 g (yield: 91.1%) of crude 1-carboxymethyl-3-chloroadamantane.

1. customwas kept at 5° -10°C
2. temperatureby external cooling
3. filtrationThe crystalline precipitate was filtered out
4. washwashed with water sufficiently
5. customair-dried