Trimethyltin chloride → 2,6-Dimethyl-4-(trimethyl-stannyl)pyridine

To a mixture of 100 g sodium (30% dispersion in toluene) and 400 ml dimethoxyethane (DME) cooled in an ice-salt bath and under nitrogen was added a solution of 121 g trimethyltin chloride in 50 ml DME over a 2 hour period while keeping the temperature below 5° C. The mixture was stirred at 0°-5° C. for 2.5 hours and then 70 g 4-chloro-2,6-dimethylpyridine in 50 ml DME was added over a 1.5 hour period while keeping the temperature at 0°-10° C. The reaction mixture was stirred at the latter temperature for 1 hour and then allowed to stand at room temperature overnight. The mixture was filtered and concentrated, and the residue treated with ether and again filtered and concentrated. The resulting orange liquid was distilled, collecting the material boiling at 130° C. (20 mm) to give 80 g 2,6-dimethyl-4-(trimethylstannyl)pyridine.

1. temperaturecooled in an ice-salt bath and under nitrogen
2. customthe temperature below 5° C
3. customat 0°-10° C
4. stirringThe reaction mixture was stirred at the latter temperature for 1 hour
5. waitto stand at room temperature overnight
6. filtrationThe mixture was filtered
7. concentrationconcentrated
8. additionthe residue treated with ether
9. filtrationagain filtered
10. concentrationconcentrated
11. distillationThe resulting orange liquid was distilled
12. customcollecting the material boiling at 130° C. (20 mm)

ORDレコード

ord-b9306a418700457a83cad69c126e58a9

出典データセット

uspto-grants-1991_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05075319