Hydrochloric Acid → HCID 21395750, compound

HRID 1439615Notes

Reaction equation

HRID 1439615 reaction equation
[C:1]1([N:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CO.[CH2:15]1[O:18][CH:16]1[CH3:17].[ClH:19]>CCOCC>[ClH:19].[OH:18][CH:16]([CH3:17])[CH2:15][N:10]1[CH2:11][CH2:12][N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:8][CH2:9]1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 887Methanol2×HCID 6378Propylene OxideHCID 70961-Phenylpiperazine

Product 1

HCID 21395750HCID 21395750, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

N-Phenylpiperazine (130 g.) was dissolved in 200 ml. methanol and the solution cooled to 0°-10° C. Propylene oxide (62 ml) was added over 5 minutes at a temperature under 10° . After the addition the cooling bath was removed. The reaction was allowed to warm to a maximum of 30° . When the reaction temperature stopped rising the solution was refluxed for 11/2 hours and then cooled. A solution of 1 mole HCl gas in 100 ml. methanol was added gradually followed by 300 ml. ether. The solid was filtered, washed with methanol-ether, then with ether to give 170 g., m. 201-5° .

Workup

  1. additionAfter the addition the cooling bath
  2. customwas removed
  3. temperatureto warm to a maximum of 30°
  4. temperaturewas refluxed for 11/2 hours
  5. temperaturecooled
  6. filtrationThe solid was filtered
  7. washwashed with methanol-ether
  8. customwith ether to give 170 g
  9. custom201-5°

Sources & evidence

ORD record
ord-5bc840c955fe4eb58e8344d95e5aa2bd
Source dataset
uspto-grants-1977_11
Patent number
US04060526

Reaction notes

Loading…