Phosphoric Acid → HCID 15087797, compound

HRID 1494635Notes

Reaction equation

HRID 1494635 reaction equation
[CH3:1][C:2]([CH3:17])([CH:4]1[CH2:9][N:8]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:7][CH2:6][NH:5]1)O.OP(O)(O)=O.[OH-].[Na+]>>[CH3:17][C:2]([CH:4]1[NH:5][CH2:6][CH2:7][N:8]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:9]1)=[CH2:1]

Participants

4

Reactant 3

HCID 1004Phosphoric AcidHCID 14798Sodium HydroxideHCID 15087796HCID 15087796, compound

Product 1

HCID 15087797HCID 15087797, compoundYield 85.6%

Conditions

Temperature
140 °C

Procedure

A mixture of 6.4 parts of α,α-dimethyl-4-(phenylmethyl)-2-piperazinemethanol and 50 parts of poly(phosphoric acid) was stirred for 1 hour at 140° C. After cooling, ice water was added and the whole was treated with a sodium hydroxide solution 50%. The product was extracted twice with dichloromethane. The combined extracts were washed with water, dried, filtered and evaporated, yielding 5 parts (85.6%) of 3-(1-methylethenyl)-1-(phenylmethyl)piperazine as a residue (int. 47).

Workup

  1. temperatureAfter cooling
  2. extractionThe product was extracted twice with dichloromethane
  3. washThe combined extracts were washed with water
  4. customdried
  5. filtrationfiltered
  6. customevaporated

Sources & evidence

ORD record
ord-cba0654288ff4072912a13f2fec856ca
Source dataset
uspto-grants-1991_06
Patent number
US05026853

Reaction notes

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