反应详情

温度

20 °C

165 ml of a 1.6 M solution of n-butyllithium in hexane was added at (-65)° C. to 170 ml of absolute tetrahydrofuran. At this temperature a solution of 61 g of dimethyl 2-methoxymethylbenzylphosphonate (from Example 8) in 100 ml of tetrahydrofuran was dripped in. After 30 minutes the batch was poured into a (-60)° C. cold saturated solution (500 ml) of dry ice and diethyl ether. After the batch had been stirred for 10 minutes it was allowed to heat up to about 20° C. over a period of 4 hours. 300 ml of water was added and the organic phase was separated off and extracted three times, each time with 100 ml of 100 ml of 10% strength sodium carbonate solution. The combined aqueous phases were extracted twice, each time with 150 ml of diethyl ether, and the pH was adjusted to 1 with 2 N sulfuric acid. Extraction was carried out three times, each time with 150 m]of dichloromethane, the organic phases were dried, and the solvent was removed under reduced pressure. There remained 60 g of dimethylphosphone-(2-methoxymethylphenyl)-acetic acid as a yellow

1. additionAfter 30 minutes the batch was poured into a (-60)° C
2. customthe organic phase was separated off
3. extractionextracted three times
4. extractionThe combined aqueous phases were extracted twice
5. extractionExtraction
6. dry with materialeach time with 150 m]of dichloromethane, the organic phases were dried
7. customthe solvent was removed under reduced pressure