1-Methylpiperazine → HCID 59313927、化合物

HRID 889438ノート

反応式

HRID 889438 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[NH2:8][C:9]1[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:10]=1[C:11](Cl)=[O:12]>C(Cl)Cl>[NH2:8][C:9]1[CH:17]=[C:16]([N+:18]([O-:20])=[O:19])[CH:15]=[CH:14][C:10]=1[C:11]([N:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)=[O:12]

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 214891672-Amino-4-nitrobenzoyl chloride

生成物 1

HCID 59313927HCID 59313927、化合物収率 52%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 1-methylpiperazine (2.5 g, 24.96 mmol) in DCM (30 mL) at 0° C. was added a solution of Intermediate 69A (1.13 g, 5.63 mmol) in DCM (10 mL) slowly. The reaction was stirred at room temperature for 1 hour. The reaction mixture was washed with saturated aqueous NaHCO3, dried over MgSO4, filtered and concentrated. The crude material was purified by flash chromatography, (SiO2, 24 g, 0-10% MeOH/DCM) to give Intermediate 69B (0.77 g, 52%) as a yellow oil. HPLC: Rt=0.360 min. (CHROMOLITH® column 4.6×50 mm eluting with 10-90% aqueous methanol over 4 min. containing 0.1% TFA, 4 mL/min., monitoring at 220 nm). MS (ES): m/z=265 [M+H]+.

後処理

  1. washThe reaction mixture was washed with saturated aqueous NaHCO3
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude material was purified by flash chromatography, (SiO2, 24 g, 0-10% MeOH/DCM)

出典と根拠

ORDレコード
ord-19e3054b587d42aeb2c5d80f10384392
出典データセット
uspto-grants-2012_08
特許番号
US08252795B2

反応ノート

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