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

HRID 1018105ノート

反応式

HRID 1018105 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-f02c7c18ec674e5ab5361e2e7e83cd84
出典データセット
uspto-grants-2002_11
特許番号
US06479672B1

反応ノート

読み込み中…