tert-Butyl piperazine-1-carboxylate → HCID 178452258, compound

HRID 501400Notes

Reaction equation

HRID 501400 reaction equation
CN(C)S([N:6]1[C:10]2[CH:11]=[N:12][N:13]([CH2:16][O:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:14](=[O:15])[C:9]=2[N:8]=[C:7]1Cl)(=O)=O.[N:27]1([C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1>>[CH2:18]([O:17][CH2:16][N:13]1[C:14](=[O:15])[C:9]2[NH:8][C:7]([N:30]3[CH2:29][CH2:28][N:27]([C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[CH2:32][CH2:31]3)=[N:6][C:10]=2[CH:11]=[N:12]1)[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

Participants

3

Reactant 2

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 594240455-Benzyloxymethyl-2-chloro-4-oxo4,5-dihydroimidazo[4,5-d]pyridazine-1-sulfonic acid dimethylamide

Product 1

HCID 178452258HCID 178452258, compoundYield 75.8%

Conditions

Temperature
150 °C

Procedure

A mixture consisting of 2.31 g of 5-benzyloxymethyl-2-chloro-4-oxo-4,5-dihydroimidazo[4,5-d]pyridazine-1-sulfonic acid dimethylamide and 4.49 g of t-butyl piperazine-1-carboxylate was heated at 150° C. under nitrogen atmosphere for 2.5 hours. The residue was purified by silica gel column chromatography. Thus, 1.94 g of the title compound was obtained from the fraction eluted with ethyl acetate.

Workup

  1. customThe residue was purified by silica gel column chromatography

Sources & evidence

ORD record
ord-a31cc5aff0174df89eb77709df78ffe0
Source dataset
uspto-grants-2010_08
Patent number
US07772226B2

Reaction notes

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