Trimethyltin chloride → 5-(Trimethylstannyl)-4-chloro-7H-pyrrolo[2,3-d]pyrimidine

温度

-78 °C

To a solution of the compound from Step A (0.92 g, 4 mmol) in THF (25 mL) was added n-BuLi (2.5 M solution in hexane, 3.48 mL) dropwise at −78° C. After the addition, the reaction mixture was stirred at −78° C. for an additional 30 min. To this solution was added trimethyltin chloride (0.88 g, 4.4 mmol) in THF (8 mL) dropwise for a period of 10 min. The reaction mixture was brought to room temperature slowly and stirred at room temperature overnight. Saturated aqueous ammonium chloride (60 mL) was added and extracted with ethyl acetate (3×70 mL). The combined organic extracts were washed with brine, dried over Na2SO4 and evaporated to dryness. The residue was purified over silica gel to give the title compound as a colorless solid.

1. additionAfter the addition
2. customwas brought to room temperature
3. stirringstirred at room temperature overnight
4. extractionextracted with ethyl acetate (3×70 mL)
5. washThe combined organic extracts were washed with brine
6. dry with materialdried over Na2SO4
7. customevaporated to dryness
8. customThe residue was purified over silica gel

ORDレコード

ord-3a54b8808b9645c2a9df29a1b12740b8

出典データセット

uspto-grants-2008_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07323453B2