Hydrochloric Acid → HCID 19956430, compound

HRID 1779554Notes

Reaction equation

HRID 1779554 reaction equation
[CH2:1]([N:4]1[CH2:9][CH2:8][CH2:7][N:6]([CH2:10]/[CH:11]=[CH:12]/[CH2:13][N:14]2[CH2:19][CH2:18][CH2:17][N:16]([CH2:20][CH2:21][CH3:22])C2)C1)[CH2:2][CH3:3].[ClH:23]>CO>[ClH:23].[ClH:23].[ClH:23].[ClH:23].[CH2:20]([NH:16][CH2:17][CH2:18][CH2:19][NH:14][CH2:13]/[CH:12]=[CH:11]/[CH2:10][NH:6][CH2:7][CH2:8][CH2:9][NH:4][CH2:1][CH2:2][CH3:3])[CH2:21][CH3:22]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 19956402HCID 19956402, compound

Product 1

HCID 19956430HCID 19956430, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 0.265 g (0.859 mmol) of (E)-1,4-bis(3-propylhexahydro-pyrimidin-1-yl)but-2-ene, 3 ml of methanol and 3.4 ml (6.8 mmol) of 2N hydrochloric acid is heated for 19 h under reflux and is then concentrated by evaporation in vacuo. Recrystallisation of the residue from methanol/water yields the title compound, m.p. >260° C. 1H-NMR (D2O): δ0.96(t,6H); 1.62-1.76(m,4H); 2.05-2.16(m,4H); 3.02(t,4H); 3.11-3.18(m,8H); 3.77(d,4H); 6.03-6.06(m,2H).

Workup

  1. temperatureis heated for 19 h
  2. temperatureunder reflux
  3. concentrationis then concentrated by evaporation in vacuo
  4. customRecrystallisation of the residue from methanol/water

Sources & evidence

ORD record
ord-78c8cb60879f408dbf8f415429b93cb2
Source dataset
uspto-grants-1997_05
Patent number
US05627215

Reaction notes

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