HRID427233

反应详情

EQUATION

反应方程式

HRID 427233 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Iodo-2′-deoxyuridine (354 mg, 1 mmol) was dissolved in 10 mL of dimethylformamide. Cuprous iodide (76 mg, 0.4 mmol), tetrakis(triphenylphosphine)palladium(0) (230 mg, 0.2 mmol), and triethylamine (200 mg, 2.0 mmol) were added. 4-Phthalimidobut-1-yne (300 mg, 1.5 mmol) was added all at once and the reaction kept at 60° C. for three hours. The clear yellow reaction was then evaporated and methylene chloride was added. Scratching of the flask induced crystallization of nearly all of the product which was filtered and recrystallized from 95% ethanol to give 335 mg (78%) of title compound as fine, feathery needles.

WORKUP

后处理

  1. customThe clear yellow reaction
  2. customwas then evaporated
  3. additionmethylene chloride was added
  4. customcrystallization of nearly all of the product which
  5. filtrationwas filtered
  6. customrecrystallized from 95% ethanol