Methyl 4-tert-butoxycarbonyl-1-(3,4,5-trimethoxybenzyl)piperazine-2-carboxylate → HCID 20066595, compound

HRID 358772Notes

Reaction equation

HRID 358772 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[C:17]([O:25][CH3:26])[CH:16]=2)[CH:10]([C:27]([O:29][CH3:30])=[O:28])[CH2:9]1)=O)(C)(C)C.[ClH:31].C(OCC)(=O)C>>[ClH:31].[ClH:31].[CH3:26][O:25][C:17]1[CH:16]=[C:15]([CH:20]=[C:19]([O:21][CH3:22])[C:18]=1[O:23][CH3:24])[CH2:14][N:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH:10]1[C:27]([O:29][CH3:30])=[O:28]

Participants

3

Reactant 2

HCID 20066667Methyl 4-tert-butoxycarbonyl-1-(3,4,5-trimethoxybenzyl)piperazine-2-carboxylateHCID 21866389Hydrogen chloride-ethyl acetate

Product 1

HCID 20066595HCID 20066595, compound

Procedure

In 4.5N HCl-ethyl acetate solution (20 ml) is dissolved methyl 4-tert-butoxycarbonyl-1-(3,4,5-trimethoxybenzyl)piperazine-2-carboxylate (5.0 g) obtained in Reference Example 19, and the solution is left standing at room temperature for 5 hours. The reaction mixture is concentrated under reduced pressure to give crystalline methyl 1-(3,4,5-trimethoxybenzyl)-piperazine-2-carboxylate dihydrochloride (4.3 g). This product is recrystallized from ethanol to afford colorless needles, m.p. 170-175° C.

Workup

  1. customobtained in Reference Example 19
  2. waitthe solution is left
  3. concentrationThe reaction mixture is concentrated under reduced pressure

Sources & evidence

ORD record
ord-55b4154227a7401bb2c71827223d4db7
Source dataset
uspto-grants-1991_03
Patent number
US04997836

Reaction notes

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