tert-Butanol → HCID 136181547, compound

Temperature

80 °C

Three millimoles of guanosine-3'-monophosphate were dissolved in a mixture of 7.5 ml of 2 N ammonia water and 5 ml of formamide, the solution was combined with 20 ml of tertiary butanol that contained 15 millimoles of dicyclohexyl carbodiimide, and the resulting mixture was heated at 80° C. for a period of 9 to 10 hours with care taken to prevent evaporation of the solvent. After the reaction, the mixture was left to stand overnight at room temperature, the precipitate was filtered off, the filtrate was concentrated under vacuum to remove the tertiary butanol, and the residue was extracted with ether. The aqueous layer was recovered, concentrated under vacuum, and the residue was treated with acetone to give a crystal of guanosine-3'-monophosphoramidate in a yield of about 50%. The crystal was heated under vacuum at 100° C. for a period of 3 to 4 hours until it was dehydrated thoroughly.

1. customevaporation of the solvent
2. customAfter the reaction
3. waitthe mixture was left
4. filtrationthe precipitate was filtered off
5. concentrationthe filtrate was concentrated under vacuum
6. customto remove the tertiary butanol
7. extractionthe residue was extracted with ether
8. customThe aqueous layer was recovered
9. concentrationconcentrated under vacuum
10. additionthe residue was treated with acetone

ORD record

ord-5b8ab559fab44be59b1a9b64a6a36ec8

Source dataset

uspto-grants-1981_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04297347