Diethyl phenylmalonate → HCID 178439991, compound

HRID 503752Notes

Reaction equation

HRID 503752 reaction equation
[NH2:1][C:2]1[N:6]=[C:5]([CH:7]([CH3:9])[CH3:8])[NH:4][N:3]=1.[C:10]1([CH:16]([C:22](OCC)=[O:23])[C:17](OCC)=[O:18])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C(N(CCCC)CCCC)CCC.[OH-].[Na+]>[CH:7]([C:5]1[N:6]=[C:2]2[N:1]=[C:17]([OH:18])[C:16]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)=[C:22]([OH:23])[N:3]2[N:4]=1)([CH3:9])[CH3:8]

Participants

5

Reactant 2

HCID 66514Diethyl phenylmalonateHCID 27564633-Amino-5-isopropyl-1,2,4-triazole

Product 1

HCID 178439991HCID 178439991, compound

Reagents, catalysts & solvents 2

HCID 7622TributylamineSolventHCID 14798Sodium HydroxideSolvent

Procedure

A solution of 5.00 g 3-amino-5-isopropyl-1,2,4-triazol and 11.24 g diethyl phenylmalonate in 18 ml N,N-dibutylbutan-1-amine is stirred at 185° C. over night. The solution is diluted with 20% w/w NaOH solution, the resulting mixture is stirred for 30 min. The aqueous layer is washed with diethylether, acidified at 0° C. with concentrated HCl until precipition of the product is complete. The precipitate is collected by filtration to yield the product, which is used without further purification.

Workup

  1. washThe aqueous layer is washed with diethylether
  2. customacidified at 0° C. with concentrated HCl until precipition of the product
  3. filtrationThe precipitate is collected by filtration
  4. customto yield the product, which
  5. customis used without further purification

Sources & evidence

ORD record
ord-880a8f58fdfe4ea9b877d6fc0490470b
Source dataset
uspto-grants-2010_08
Patent number
US07776864B2

Reaction notes

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