反应详情

A solution of sodium nitrite (1.28 g) in water (8 ml) was added over 10 min to a mixture of methyl 3-amino-4-chlorobenzoate (4.0 g) in water (40 ml) and concentrated hydrochloric acid (5 ml) at 0° C. After 30 min the mixture was neutralised with aqueous sodium hydroxide solution to pH˜7 then added portionwise to a solution of copper cyanide (prepared from sodium cyanide (2.87 g) and copper(I) chloride (2.23 g) in water (40 ml)) at 0° C. The mixture was stirred at room temperature for 2 h then partitioned between ethyl acetate and water. The organics were washed with water, dried and evaporated under reduced pressure. The residue was triturated with 20% ethyl acetate/isohexane to yield a solid (1.55 g).

1. customthen partitioned between ethyl acetate and water
2. washThe organics were washed with water
3. customdried
4. customevaporated under reduced pressure
5. customThe residue was triturated with 20% ethyl acetate/isohexane