Iodine → HCID 67606162、化合物

Anhydrous tetrahydrofuran (125 mL) was put into a reactor with magnesium (5.7 g, 0.24 mol) and molecular sieves 4A which had been dehydrated and deaerated, followed by charging of argon gas. A small amount of iodine was slowly added to the mixture. (S)-(+)-1-bromo-2-methylbutane (30 g, 0.20 mol) was added dropwise to the slowly stirred mixture so that the reaction mixture was gradually refluxed. After the reaction was complete, the obtained Grignard reagent was transferred to a dropping funnel. The Grignard reagent was added dropwise to a solution being stirred containing phenyltrichlorosilane (50 g, 0.24 mol) in anhydrous tetrahydrofuran (50 mL) in another reactor which had been dehydrated and deaerated, followed by charging of argon gas, at 40° C.-50° C. The reaction mixture was then stirred overnight at room temperature. Hexane (500 mL) was added to the reaction mixture, and the resulting mixture was filtered under pressure, followed by fractional distillation of the filtrate to provide the desired product.

1. temperaturewas gradually refluxed
2. customby charging of argon gas, at 40° C.-50° C
3. stirringThe reaction mixture was then stirred overnight at room temperature
4. filtrationthe resulting mixture was filtered under pressure
5. distillationfollowed by fractional distillation of the filtrate

ORDレコード

ord-68b0b1270932435b9b009a92f1bad50d

出典データセット

uspto-grants-1998_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05710301