Tributyltin Chloride → 2-(Diethoxymethyl)-5-(tributylstannyl) thiophene

温度

-78 °C

18.6 g (100 mmol) of 2-(diethoxymethyl) thiophene in 100 ml of tetrahydrofuran ("THF") was placed in a 2-neck flask equipped with dropping funnel. The solution was cooled to -78° C. under nitrogen atmosphere and added 62.5 mL of 1.6 M n-butyl lithium (100 mmol) dropwise through dropping funnel in 1 hr. The reaction mixture was stirred at -78° C. for 1 hr and gradually warmed up to room temperature. After stirred for 30 minutes, the mixture was again cooled to -78° C. and added dropwise a THF (50 mL) solution of 32.5 g (100 mmol) of tributyl tin chloride with continual stirring. Gradually warmed up to room temperature, the mixture was stirred for another 10-12 hrs at room temperature and then concentrated. Reduced pressure distillation yielded 36.8 g (80%) of 2-(diethoxymethyl)-5-(tributylstannyl) thiophene (bp 195° C./1 torr).

1. customequipped
2. customin 1 hr
3. temperaturegradually warmed up to room temperature
4. stirringAfter stirred for 30 minutes
5. temperaturethe mixture was again cooled to -78° C.
6. temperatureGradually warmed up to room temperature
7. stirringthe mixture was stirred for another 10-12 hrs at room temperature
8. concentrationconcentrated
9. distillationReduced pressure distillation

ORDレコード

ord-c01d9dfaaaf344c0bc5c37c21112a344

出典データセット

uspto-grants-1999_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05994394