Propionic Acid → HCID 13518799, compound

HRID 370449Notes

Reaction equation

HRID 370449 reaction equation
[Cl:1][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]([NH:12][NH2:13])=[N:4][N:3]=1.[C:14](O)(=O)[CH2:15][CH3:16]>>[Cl:1][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[C:14]([CH2:15][CH3:16])[N:4]2[N:3]=1

Participants

3

Reactant 2

HCID 1032Propionic AcidHCID 640098866597-78-2

Product 1

HCID 13518799HCID 13518799, compoundYield 89.6%

Procedure

A solution of 98.5 grams (0.496 mole) of 1-chloro-4-hydrazino-5,6,7,8-tetrahydrophthalazine in 300 milliliters of propionic acid was heated at reflux for 18 hours, then concentrated by evaporation to half the original volume. The solution was diluted with aqueous sodium carbonate until neutral (pH 7). The resulting precipitate was collected, air-dried at ambient temperature, then dried in a drying over to produce 105 grams (0.444 mol) of 6-chloro-3-ethyl-7,8,9,10-tetrahydro-1,2,4-triazolo[3,4-a]phthalazine, melting at 93°-94° C. (89.6% yield). Calculated for C11H13ClN4 : C, 55.81; H, 5.53; N, 23.67. Found: C, 56.00; H, 5.63; N, 23.87.

Workup

  1. temperatureat reflux for 18 hours
  2. concentrationconcentrated by evaporation to half the original volume
  3. additionThe solution was diluted with aqueous sodium carbonate until neutral (pH 7)
  4. customThe resulting precipitate was collected
  5. customair-dried at ambient temperature
  6. customdried in a drying over

Sources & evidence

ORD record
ord-07b037e839e44e479582330e090c8db5
Source dataset
uspto-grants-1985_07
Patent number
US04526890

Reaction notes

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