HCID 66879199, compound → HCID 178468818, compound

HRID 1913215Notes

Reaction equation

HRID 1913215 reaction equation
C(O[C:4](=[O:20])[CH2:5][C:6](=O)[CH2:7][CH:8]1[CH2:13][CH2:12][CH:11]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:10][CH2:9]1)C.[NH2:21][C:22]1[CH:26]=[CH:25][NH:24][N:23]=1>CCO>[OH:20][C:4]1[N:23]2[N:24]=[CH:25][CH:26]=[C:22]2[N:21]=[C:6]([CH2:7][CH:8]2[CH2:9][CH2:10][CH:11]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:12][CH2:13]2)[CH:5]=1

Participants

4

Reactant 2

HCID 66879199HCID 66879199, compoundHCID 178418806HCID 178418806, compound

Product 1

HCID 178468818HCID 178468818, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
100 °C

Procedure

To a 50 mL round-bottom flask containing ethyl 4-(4-ethoxy-2,4-dioxobutyl)cyclohexanecarboxylate (Int-4e, 2.33 g, 8.19 mmol) was added 3-amino-1H-pyrazole (681 mg, 8.19 mmol). The flask was heated via heat gun to ensure mixing of the oils, and then the reaction was shaken at 100° C. for 18 hours. After 18 hours, the resulting solid was taken up in EtOH and then the solvent was removed in vacuo to dry product. The product was then pumped dry on high vacuum overnight to further dry the product. The compound was taken on without further purification.

Workup

  1. temperatureThe flask was heated
  2. temperaturevia heat gun
  3. additionto ensure mixing of the oils
  4. waitAfter 18 hours
  5. customthe solvent was removed in vacuo to dry product
  6. customThe product was then pumped dry on high vacuum overnight
  7. customto further dry the product
  8. customThe compound was taken on without further purification

Sources & evidence

ORD record
ord-86c4127d0e6a40f7922627b45bcfc556
Source dataset
uspto-grants-2013_12
Patent number
US08609675B2

Reaction notes

Loading…