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

HRID 1018105

반응식

HRID 1018105 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-f02c7c18ec674e5ab5361e2e7e83cd84
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06479672B1

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