反应详情

312 mg of 3-hydroxythiophene, 380 mg of 2,6-dichloropurine, 6 ml of tetrahydrofuran, 786 mg of triphenylphosphine (P(phenyl)3) are mixed together at ambient temperature then 0.47 ml of DEAD (diethyl-azodicarboxylate) is added over 10 minutes and agitation is carried out overnight at ambient temperature. Then 10 ml of NaH2PO4 in aqueous solution 1M is added, followed by extracting 3 times with 10 ml of methylene chloride, washing with 10 ml of water with 5 of an aqueous solution of sodium chloride, drying and evaporating to dryness. After purification on silica eluting with methylene chloride/ethyl acetate in a proportion of 75/25 then 90/10, impasting is carried out at ambient temperature in 5 ml of isopropyl ether, followed by separating, washing with 5 ml of isopropyl ether and drying at ambient temperature. In this way 137 mg of expected product is obtained in the form of white crystals.

1. extractionby extracting 3 times with 10 ml of methylene chloride
2. washwashing with 10 ml of water with 5 of an aqueous solution of sodium chloride
3. customdrying
4. customevaporating to dryness
5. customAfter purification on silica eluting with methylene chloride/ethyl acetate in a proportion of 75/25
6. customis carried out at ambient temperature in 5 ml of isopropyl ether
7. customby separating
8. washwashing with 5 ml of isopropyl ether
9. customdrying at ambient temperature