Piperazine → HCID 131723977, compound

HRID 1296610Notes

Reaction equation

HRID 1296610 reaction equation
[Cl:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]([O:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])[N:3]=1.[NH:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.C([O-])([O-])=O.[K+].[K+]>>[ClH:1].[ClH:1].[CH3:17][O:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[CH2:9][O:8][C:4]1[CH:5]=[N:6][CH:7]=[C:2]([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)[N:3]=1

Participants

4

Reactant 3

HCID 4837PiperazineHCID 11430Potassium CarbonateHCID 18186809HCID 18186809, compound

Product 1

HCID 131723977HCID 131723977, compound

Procedure

The title compound was prepared according to the procedure of example 4, step 2 starting from the product of step 1 above (0.49 g), piperazine (0.86 g, 10 mmol) and K2CO3 (1.00 g, 7.2 mmol). This gave the free base of the title compound as an oil. Yield 0.43 g (73%). The free base was dissolved in ethyl ether and a solution of HCl in diethyl ether was added until no more precipitate was formed. The precipitate was collected, washed with diethyl ether, and dried in vaccum to give 0.41 g (56%) of the title compound: mp 171-173° C.). HRMS m/z calcd for C16H20N4O2 (M)+ 300.1586, found 300.1586. Anal. (C16H20N4O2.2HCl) C, H, N.

Workup

  1. customThe title compound was prepared

Sources & evidence

ORD record
ord-1ad7d704ebb84f89b629509b41ec5ee9
Source dataset
uspto-grants-2007_07
Patent number
US07247633B2

Reaction notes

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