Phosphorus oxychloride → HCID 131730134, compound

HRID 1798945Notes

Reaction equation

HRID 1798945 reaction equation
[CH:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10]2[CH:11]=[CH:12][C:13](=O)[NH:14][N:15]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].O=P(Cl)(Cl)[Cl:19]>>[ClH:19].[Cl:19][C:13]1[N:14]=[N:15][C:10]([CH:7]2[CH2:8][CH2:9][N:4]([CH:1]([CH3:3])[CH3:2])[CH2:5][CH2:6]2)=[CH:11][CH:12]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 68495857HCID 68495857, compound

Product 1

HCID 131730134HCID 131730134, compoundYield 88%

Conditions

Temperature
60 °C

Procedure

6-(1-Isopropylpiperidin-4-yl)pyridazin-3-on (5.76 g, 26 mmol) was added to POCl3 (50 mL) and the reaction mixture was heated for 2 hours at 60° C. The excess of POCl3 was evaporated in vacuo and ethanol (96%) was added under an exothermic reaction. The reaction mixture was cooled and a precipitate was obtained. The product was filtered off after drying in vacuo and 6.34 g (88%) white crystals were isolated.

Workup

  1. customThe excess of POCl3 was evaporated in vacuo and ethanol (96%)
  2. additionwas added under an exothermic reaction
  3. temperatureThe reaction mixture was cooled
  4. customa precipitate was obtained
  5. filtrationThe product was filtered off
  6. customafter drying in vacuo

Sources & evidence

ORD record
ord-d7730c9bd61244dda556684e9c298ef3
Source dataset
uspto-grants-2013_01
Patent number
US08344001B2

Reaction notes

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