Hydrochloric Acid → 1255099-59-2

HRID 1993645Notes

Reaction equation

HRID 1993645 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][N:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>>[ClH:20].[Cl:20][C:18]1[CH:17]=[CH:16][N:15]=[C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)[CH:19]=1

Participants

3

Reactant 2

HCID 313Hydrochloric Acid2×HCID 68535175HCID 68535175, compound

Product 1

HCID 685418771255099-59-2

Procedure

Treat a room temperature solution of 4-(4-chloro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (0.6 g, 1.9 mmol) in CH2CL2 (4 mL) with HCl (4 N solution in dioxane, 1.5 mL, 5.9 mmol) resulting in a slight exotherm. Stir the mixture for 3 hours, add additional HCl (4 N solution in dioxane, 1.5 mL, 5.9 mmol), and stir overnight. Concentrate under reduced pressure to afford 1-(4-chloro-pyridin-2-yl)-piperazine hydrochloride, then titurate with Et2O (0.43 g). LCMS ES+(m/z) 198 [M+H]).

Workup

  1. customresulting in a slight exotherm
  2. stirringstir overnight
  3. concentrationConcentrate under reduced pressure

Sources & evidence

ORD record
ord-8649051addba4dcea2cff57992ac48ff
Source dataset
uspto-grants-2010_01
Patent number
US07652015B2

Reaction notes

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