1-Butanol → HCID 58757226, compound

Participants

Reaction Steps

The product from Step 3 (2 g, 5.9 mmol) was suspended in 12 N HCl (35 mL) and n-butanol (35 mL) and the mixture heated at 100° C. for 7 h and then allowed to cool to room temperature. The reaction mixture was evaporated to dryness in vacuo, and then partitioned between 2 N NaOH (50 mL) and dichloromethane (50 mL). The organic layer was separated and found to contain some unreacted starting material only and was discarded, while the aqueous layer was neutralized with concentrated HCl and the resulting precipitate collected by filtration and washed with ethyl acetate to give 6-amino-9-benzyl-2-chloro-7,9-dihydro-purin-8-one as an off-white solid (1.5 g, 94%) which was found to be >90% pure and was used with no further purification.

Provenance & Evidence