Phosphorus oxychloride → HCID 86698298, compound
Reaction equation
[CH2:1]([C:3]1[C:11]2[C:10](=O)[NH:9][CH:8]=[N:7][C:6]=2[Se:5][C:4]=1[CH3:13])[CH3:2].P(Cl)(Cl)([Cl:16])=O>>[Cl:16][C:10]1[C:11]2[C:3]([CH2:1][CH3:2])=[C:4]([CH3:13])[Se:5][C:6]=2[N:7]=[CH:8][N:9]=1Participants
3
Procedure
A mixture of 5-ethyl-6-methylselenopheno[2,3-d]pyrimidin-4(3H)-one (300 mg) and phosphorous oxychloride (5 mL) was refluxed for 1 h. The reaction mixture was attained to rt and poured into ice cold water and stirred for 10 min. The precipitated solid was filtered, washed with water and dried to give the product as a brown color solid (260 mg, 81%), mp 58-60° C. 1H NMR (400 MHz, CDCl3): δ 8.68 (1H, s), 3.06 (2H, q, J=7.5 Hz), 2.62 (3H, s), 1.23 (3H, t, J=7.4 Hz).
Workup
- temperaturewas refluxed for 1 h
- customwas attained to rt
- additionpoured into ice cold water
- filtrationThe precipitated solid was filtered
- washwashed with water
- customdried
Sources & evidence
- ORD record
- ord-c0258d0f0f3c4b41a1dcaaf8f541278e
- Source dataset
- uspto-grants-2014_08
- Patent number
- US08815879B2
Reaction notes
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