1H-1,2,4-Triazole → HCID 19914728, compound

HRID 1090177Notes

Reaction equation

HRID 1090177 reaction equation
[NH:1]1[CH:5]=[N:4][CH:3]=[N:2]1.C([O-])([O-])=O.[K+].[K+].CS(O[CH2:17][O:18][C:19](=[O:28])[CH2:20][C:21]1[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][CH:22]=1)(=O)=O.CCCCCC.C(O)C>CC(C)=O>[N:1]1([CH:20]([C:21]2[CH:22]=[CH:23][C:24]([Cl:27])=[CH:25][CH:26]=2)[C:19]([O:18][CH3:17])=[O:28])[CH:5]=[N:4][CH:3]=[N:2]1

Participants

6

Conditions

Temperature
10 °C

Procedure

A suspension of 3.2 g of 1,2,4-triazole and 8.3 g of K2CO3 in 300 ml of anhydrous acetone is refluxed over 1 hour. After cooling to 10° C., 14 g of methyl α-(methanesulphonyloxymethyl-4-chlorophenyl-acetate is added. The temperature is then allowed to spontaneously rise to room temperature, and the reaction mixture is stirred for one hour, is filtered over fritted glass and the filtrate is concentrated under vacuum, 13 g thus being obtained of raw solid product, which is suspended with 10 ml of 1:1 n-hexane+ethanol mixture.

Workup

  1. temperatureis refluxed over 1 hour
  2. customto spontaneously rise to room temperature
  3. filtrationis filtered over fritted glass
  4. concentrationthe filtrate is concentrated under vacuum, 13 g
  5. customthus being obtained of raw solid product, which

Sources & evidence

ORD record
ord-4a302005ac1e4e5c94e59b5d098753c4
Source dataset
uspto-grants-1992_01
Patent number
US05081141

Reaction notes

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