2-Methylpiperazine → (RS)-4-(3-methylpiperazin-1-yl)benzamide

HRID 849499

反応式

HRID 849499 の反応式
F[C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][CH:3]=1.[CH3:11][CH:12]1[CH2:17][NH:16][CH2:15][CH2:14][NH:13]1>O>[CH3:11][CH:12]1[NH:13][CH2:14][CH2:15][N:16]([C:2]2[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][CH:3]=2)[CH2:17]1

参加物

4

反応物 2

HCID 660572-MethylpiperazineHCID 715724-Fluorobenzamide

生成物 1

HCID 19367109(RS)-4-(3-methylpiperazin-1-yl)benzamide収率 87.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
100 °C

実験手順

A mixture of 4-fluorobenzamide (Aldrich; 2.432 g), (RS)-2-methylpiperazine (Aldrich; 4.247 g), and water (9 mL) is heated at 100° C. for 7 days. The mixture is then cooled to 41° C. and water is added. The solid is collected, washed with water and toluene and dried under reduced pressure to give 3.37 g of (RS)-4-(3-methylpiperazin-1-yl)benzamide; 1H NMR (CDCl3, CD3OD) δ 1.17, 2.48, 2.82, 2.94-3.15, 3.04, 3.68, 6.89, 7.73.

後処理

  1. temperatureThe mixture is then cooled to 41° C.
  2. customThe solid is collected
  3. washwashed with water and toluene
  4. customdried under reduced pressure

出典と根拠

ORDレコード
ord-6e947ac27ebe459d931f683fc1d796c6
出典データセット
uspto-grants-2000_01
特許番号
US06013654

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