Formamide → HCID 178518069, compound

Temperature

200 °C

A mixture of ethyl 2-amino-4-(2-furyl)thiophene-3-carboxylate (1.00 g, 4.21 mmol) and formamide (10.0 g, 0.2 mol) was warmed by microwave at 200° C. for 10 minutes. The mixture was concentrated in vacuo at 90° C., diluted with 40 mL of 10% methanol/dichloromethane, and filtered through a 40 gram silica gel column using 5% methanol/dichloromethane to wash the material through the column. The filtrate was again concentrated and the remaining residue was purified by column chromatography over silica gel using a gradient elution from 5 to 10% methanol in dichloromethane to give 0.482 g (52.4%) of 4-hydroxy-5-(2-furyl)thieno[2,3-d]pyrimidine as a brown solid.

1. concentrationThe mixture was concentrated in vacuo at 90° C.
2. additiondiluted with 40 mL of 10% methanol/dichloromethane
3. filtrationfiltered through a 40 gram silica gel column
4. washto wash the material through the column
5. concentrationThe filtrate was again concentrated
6. customthe remaining residue was purified by column chromatography over silica gel using
7. washa gradient elution from 5 to 10% methanol in dichloromethane

ORD record

ord-b04b88601bd942269bcdb9305aedafe7

Source dataset

uspto-grants-2009_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07576080B2