Acetone → HCID 19417509、化合物

反応式

Cl.[Cl:2][C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][C:9]=1[O:10][CH3:11])[NH2:6].[C:12]([NH:14][C:15]([NH2:17])=[NH:16])#[N:13].[CH3:18][C:19]([CH3:21])=O>>[ClH:2].[Cl:2][C:3]1[CH:4]=[C:5]([N:6]2[C:19]([CH3:21])([CH3:18])[N:16]=[C:15]([NH2:17])[N:14]=[C:12]2[NH2:13])[CH:7]=[CH:8][C:9]=1[O:10][CH3:11]

参加物

反応物 3

HCID 180Acetone

HCID 122278893-Chloro-4-methoxyaniline hydrochloride

HCID 178418324HCID 178418324、化合物

生成物 1

HCID 19417509HCID 19417509、化合物

実験手順

A stirred mixture of 3.0 grams (0.019 mole) of 90% pure 3-chloro-4-methoxyaniline and 4 mL of concentrated hydrochloric acid in 20 mL of toluene was heated to reflux using a heat gun. The reaction mixture was then concentrated under reduced pressure to a residue. The residue was triturated with 50 mL of diethyl ether, and the resultant solid was collected by filtration. The solid was dried under vacuum, yielding 3.4 grams (0.018 mole) of 3-chloro-4-methoxyaniline hydrochloride. A stirred mixture of the aniline hydrochloride and 1.8 grams (0.022 mole) of cyanoguanidine in 25 mL of acetone was then heated at reflux for about 20 hours. The mixture was cooled, and a solid was collected by filtration. The solid was dried under vacuum, yielding 4.9 grams of 1-(3-chloro-4-methoxyphenyl)-2,4-diamino-6,6-dimethyl-1,6-dihydro-1,3,5-triazine hydrochloride, mp 232 ° C. The NMR spectrum was consistent with the proposed structure.