反应详情

温度

90 °C

A suspension of tetrazolo[1,5-a][1,7]naphthyridin-5-ol (3.5 g) in phosphorous oxychloride (15 mL) was heated at 90° C. for 2 hours. The reaction mixture was concentrated under vacuum. The residue was poured into ice water, dichloromethane was added followed by the addition of 10% sodium hydroxide to neutral pH. The product was partitioned into dichloromethane. The dichloromethane layer was separated, dried over magnesium sulfate then concentrated under vacuum to provide 3.8 g of 5-chlorotetrazolo[1,5-a][1,7]naphthyridine as a solid, m.p. 176-177° C. Analysis: Calculated for C8H4ClN5: %C, 46.73; %H, 1.96; %N, 34.06; Found: %C, 46.80; %H, 2.16; %N, 34.45.

1. concentrationThe reaction mixture was concentrated under vacuum
2. additionThe residue was poured into ice water, dichloromethane
3. additionwas added
4. additionfollowed by the addition of 10% sodium hydroxide to neutral pH
5. customThe product was partitioned into dichloromethane
6. customThe dichloromethane layer was separated
7. dry with materialdried over magnesium sulfate
8. concentrationthen concentrated under vacuum