Hydrochloric Acid → HCID 974966、化合物

反応式

[F:1][C:2]1[CH:15]=[CH:14][CH:13]=[CH:12][C:3]=1[C:4]([NH:6][NH:7][C:8]([NH:10][CH3:11])=[S:9])=O.Cl.N1C=CC=CC=1.C([O-])(O)=O.[Na+].Cl>>[F:1][C:2]1[CH:15]=[CH:14][CH:13]=[CH:12][C:3]=1[C:4]1[N:10]([CH3:11])[C:8](=[S:9])[NH:7][N:6]=1

参加物

反応物 4

HCID 313Hydrochloric Acid

HCID 516892Sodium Bicarbonate

HCID 34380302-(2-fluorobenzoyl)-N-methyl-1-hydrazinecarbothioamide

HCID 10176127Pyridinium chloride

生成物 1

HCID 974966HCID 974966、化合物

実験手順

1-(2-Fluorobenzoyl)-4-methylthiosemicarbazide (11.3 g, 4.97×10-2 mole) or the aforementioned mixture of the above and pyridine hydrochloride and 1 molar aqueous NaHCO3 (480 ml, 4.80×10-1 mole) were stirred and heated to reflux. After refluxing overnight, the reaction was cooled in an ice bath before being acidified by the dropwise addition of concentrated hydrochloric acid (40 ml, 4.8×10-1 mole). The resulting precipitate was collected by filtration, washed with a little H2O, and dried by suction. This afforded a colorless powder: 5.0 g (48%). This material was of sufficient purity to go on to the next step. If desired this material could be crystallized from EtOAc/hexane affording colorless needles, mp 137°-139° C.