Pentane → Stannane, trimethyl-2-thienyl-

Temperature

-38 °C

To a solution of thiophene (2.1 g, 25.0 mmol) in anhydrous THF (50 mL) was added dropwise over 30 minutes at −38° C. t-butyllithium in pentane (1.6 M, 16.0 mL, 25.6 mmol). The solution was stirred for 1 h at −38° C. and then cooled to −78° C. Trimethyltin chloride in THF (1 M, 25.3 mL, 25.3 mmol) was added dropwise over 30 min. The reaction was then stirred for 2 h at −78° C. and then for 15 h at r.t. The solvent was evaporated and the resulting yellow solid was taken up in other, washed with water and dried Na2SO4 and then evaporated to give a light brown liquid which solidified on standing.

1. temperaturecooled to −78° C
2. stirringThe reaction was then stirred for 2 h at −78° C.
3. waitfor 15 h at r.t
4. customThe solvent was evaporated
5. washwashed with water and dried Na2SO4
6. customevaporated
7. customto give a light brown liquid which

ORD record

ord-afba8c43295f4fbaa3a1cd1f053a1d5d

Source dataset

uspto-grants-2005_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06875593B2