4,6-Dichloropyrimidine → HCID 53257559, compound

Participants

Reaction Steps

1.077 g 3-Indol-1-ylmethyl-phenylamine (obtained in Step 2, 4.84 mmol) and 0.722 g 4,6-dichloropyrimidine (4.84 mmol) was dissolved in 50 cm3 of isopropyl-alcohol, 1.27 cm3 N,N-diisopropyl-ethylamine (0.939 g, 7.27 mmol) were added and the mixture was refluxed for three days. Then the mixture was evaporated under reduced pressure, 100 cm3 of water was added and it was extracted with 3×70 cm3 ethyl-acetate. Combined organic layer was washed with brine, dried over MgSO4 and evaporated to a yellowish oil. The residue was crystallized from minimal amount of acetonitrile and washed with diethyl-ether to give the desired product as an off-white solid. Overall yield for Step 2 and Step 3: 1.015 g (63%). For analitical results and compound identification see Table 1. The compound was used as a starting material in the preparation of Example 91.

Provenance & Evidence