1-Methylpiperazine → HCID 59313927, 화합물

HRID 889438노트

반응식

HRID 889438 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 59313927HCID 59313927, 화합물수율 52%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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]+.

후처리

  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)

출처 및 근거

ORD 기록
ord-19e3054b587d42aeb2c5d80f10384392
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252795B2

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