Tetrahydrofuran → Zinc(II)Chloride.1-[2-(Dimethylamino)ethyl]-4-methylpiperazine

HRID 1018105Notes

Reaction equation

HRID 1018105 reaction equation
[Cl-:1].[Zn+2:2].[Cl-].O1CCCC1.[CH3:9][N:10]([CH3:20])[CH2:11][CH2:12][N:13]1[CH2:18][CH2:17][N:16]([CH3:19])[CH2:15][CH2:14]1>>[Cl-:1].[Zn+2:2].[Cl-:1].[CH3:9][N:10]([CH3:20])[CH2:11][CH2:12][N:13]1[CH2:14][CH2:15][N:16]([CH3:19])[CH2:17][CH2:18]1

Participants

4

Reactant 3

HCID 8028TetrahydrofuranHCID 669081-(2-(N,N-Dimethylamino)ethyl)-4-methylpiperazineHCID 3007855Zincchloride

Product 1

HCID 9861400Zinc(II)Chloride.1-[2-(Dimethylamino)ethyl]-4-methylpiperazine

Procedure

To a solution of zinc (II) chloride in tetrahydrofuran(0.5M, 300 mL, 150 mmol) was added dropwise 1-[2-(dimethylamino)ethyl]-4-methylpiperazine (38.54 g, 225 mmol) below 20° C. under nitrogen atmosphere. The slurry was stirred at room temperature for 4 hrs., and filtered under nitrogen flow. The cake was washed with dry tetrahydrofuran(100 mL), and dried at room temperature under reduced pressure overnight. The title compound (47.56 g, quantitative yield) was obtained as colorless crystals. mp: ca. 260° C.(dec.). IR(KBr, cm−1): 3,430; 2,960; 2,870; 2,820; 1,490; 1,330; 1,190; 1,140; 1,040; 990; 860

Workup

  1. filtration, and filtered under nitrogen flow
  2. washThe cake was washed with dry tetrahydrofuran(100 mL)
  3. customdried at room temperature under reduced pressure overnight

Sources & evidence

ORD record
ord-f02c7c18ec674e5ab5361e2e7e83cd84
Source dataset
uspto-grants-2002_11
Patent number
US06479672B1

Reaction notes

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