Diethyl phenylmalonate → HCID 178517387, compound

HRID 1915530Notes

Reaction equation

HRID 1915530 reaction equation
[NH:1]1[CH:5]=[N:4][C:3]([NH2:6])=[N:2]1.[C:7]1([CH:13]([C:19](OCC)=[O:20])[C:14](OCC)=[O:15])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(N(CCCC)CCCC)CCC.[OH-].[Na+]>[C:7]1([C:13]2[C:14]([OH:15])=[N:6][C:3]3[N:2]([N:1]=[CH:5][N:4]=3)[C:19]=2[OH:20])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Participants

5

Reactant 2

HCID 66514Diethyl phenylmalonateHCID 178418311HCID 178418311, compound

Product 1

HCID 178517387HCID 178517387, compound

Reagents, catalysts & solvents 2

HCID 7622TributylamineSolventHCID 14798Sodium HydroxideSolvent

Procedure

A solution of 10 g 1,2,4-triazol-3-amine and 33.7 g diethyl phenylmalonate in N,N-dibutylbutan-1-amine is stirred at 185° C. over night. The solution is diluted with 10% w/w NaOH solution, the resulting mixture is stirred for 30 min and the organic phase is separated. The aqueous layer is extracted with diethylether, acidified with concentrated HCl until precipition of the product is complete and the precipitate collected by filtration to yield the product, which is used without further purification.

Workup

  1. customthe organic phase is separated
  2. extractionThe aqueous layer is extracted with diethylether
  3. filtrationthe precipitate collected by filtration
  4. customto yield the product, which
  5. customis used without further purification

Sources & evidence

ORD record
ord-3a0a727a00b840ff86e92d9a3dff080f
Source dataset
uspto-grants-2013_12
Patent number
US08614218B2

Reaction notes

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