反应详情

温度

0 °C

A solution of 0.53 ml of acryloyl chloride in 3 ml of methylene chloride is slowly added dropwise at 0° C. to a solution of 0.78 g of phthalazine and 1.2 ml of 1-trimethylsiloxy-cyclohexene. After the addition the mixture is stirred at 0° C. for a further 30 min., then concentrated, treated with ice-water and made basic by the addition of sodium carbonate. The mixture is extracted 3 times with 100 ml of ethyl acetate each time. The organic phases are combined, dried over magnesium sulphate, filtered and the filtrate is concentrated. 1.63 g of (RS)-2-(2-acryloyl-1,2-dihydro-phthalazin-1-yl)-cyclohexanone (mixture of diastereomers) are isolated as a brownish oil. MS: 282 (M+).

1. additionAfter the addition the mixture
2. concentrationconcentrated
3. additiontreated with ice-water
4. additionmade basic by the addition of sodium carbonate
5. extractionThe mixture is extracted 3 times with 100 ml of ethyl acetate each time
6. dry with materialdried over magnesium sulphate
7. filtrationfiltered
8. concentrationthe filtrate is concentrated