Monobasic potassium phosphate → HCID 686817, compound

Reaction equation

P([O-])(O)(O)=O.[K+].[Cl:7][C:8]1[CH:9]=[C:10]([C:14]2([NH:18]C(OCC(Cl)(Cl)Cl)=O)[CH2:17][CH2:16][CH2:15]2)[CH:11]=[CH:12][CH:13]=1>C1COCC1.[Zn]>[Cl:7][C:8]1[CH:9]=[C:10]([C:14]2([NH2:18])[CH2:17][CH2:16][CH2:15]2)[CH:11]=[CH:12][CH:13]=1

Participants

Procedure

According to the procedure of Just and Grozinger (Just, G. and K. Grozinger, Synthesis 457 (1976)), a rapidly stirring mixture of 1.0 ml of 1M potassium dihydrogenphosphate and Zn powder (1.0 g) was treated dropwise during 1 minute with a solution of the product from Step 3 in 5 ml of THF. After 10 minutes, an exotherm to 28° C. was produced and the two-phase system gave way to a slurry. This mixture was stirred for 1 hour when it was filtered through celite; the filter cake was washed alternately with THF and H2O (twice each). The pooled filtrate was concentrated in vacuo and the aqueous residue was cooled and brought to pH 12-13 with 8% aqueous NaOH. This was extracted 3 times with CHCl3 ; the extracts were washed with H2O and then with brine. The pooled extract was dried (MgSO4) and concentrated to give 0.23 g (92%) of the titled product.