Hydrochloric Acid → N-(1-methylethyl)-N-((2R)-2-piperazinylmethyl)methanesulfonamide dihydrochloride

HRID 1972610Notes

Reaction equation

HRID 1972610 reaction equation
[CH3:1][CH:2]([N:4]([CH2:9][C@H:10]1[CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12][N:11]1C(OC(C)(C)C)=O)[S:5]([CH3:8])(=[O:7])=[O:6])[CH3:3].[ClH:30]>CCOC(C)=O>[ClH:30].[ClH:30].[CH3:3][CH:2]([N:4]([CH2:9][C@H:10]1[CH2:15][NH:14][CH2:13][CH2:12][NH:11]1)[S:5]([CH3:8])(=[O:6])=[O:7])[CH3:1]

Participants

4

Conditions

Temperature
70 °C

Procedure

A 150-mL round-bottomed flask was charged with di-tert-butyl (2R)-2-(((1-methylethyl)(methylsulfonyl)amino)methyl)-1,4-piperazinedicarboxylate (0.617 g, 1.42 mmol), HCl (4.0 M in 1,4-dioxane, 2.80 mL, 11.2 mmol) and EtOAc (20 mL). The mixture was heated at 70° C. for 18 h. The reaction mixture was allowed to cool to room temperature and the resulting white solid was collected by filtration. The solid was washed with EtOAc and to obtain N-(1-methylethyl)-N-((2R)-2-piperazinylmethyl)methanesulfonamide dihydrochloride (0.421 g) as a white solid.

Workup

  1. temperatureto cool to room temperature
  2. filtrationthe resulting white solid was collected by filtration
  3. washThe solid was washed with EtOAc

Sources & evidence

ORD record
ord-3ea682e7cf0f4ba68cc234b8441049a9
Source dataset
uspto-grants-2013_04
Patent number
US08431563B2

Reaction notes

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