Potassium Carbonate → 4-chloro-N-methyl-2-nitro-5-(3-(trifluoromethyl)piperidin-1-yl)aniline

HRID 1258627

반응식

HRID 1258627 반응식
[F:1][C:2]([F:10])([F:9])[CH:3]1[CH2:8][CH2:7][CH2:6][NH:5][CH2:4]1.C(=O)([O-])[O-].[K+].[K+].[Cl:17][C:18]1[C:25](Cl)=[CH:24][C:21]([NH:22][CH3:23])=[C:20]([N+:27]([O-:29])=[O:28])[CH:19]=1>CN(C=O)C>[Cl:17][C:18]1[C:25]([N:5]2[CH2:6][CH2:7][CH2:8][CH:3]([C:2]([F:10])([F:9])[F:1])[CH2:4]2)=[CH:24][C:21]([NH:22][CH3:23])=[C:20]([N+:27]([O-:29])=[O:28])[CH:19]=1

참가 물질

5

반응물 3

HCID 11430Potassium Carbonate2회HCID 2893174,5-Dichloro-n-methyl-2-nitroanilineHCID 27607763-(Trifluoromethyl)piperidine

생성물 1

HCID 441206424-chloro-N-methyl-2-nitro-5-(3-(trifluoromethyl)piperidin-1-yl)aniline

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

3-(Trifluoromethyl)piperidine (0.69 g, 4.5 mmol) followed by potassium carbonate (1.25 g, 9.1 mmol) were added to 4,5-dichloro-N-methyl-2-nitroaniline (1.00 g, 4.5 mmol) in DMF (15 mL). The reaction mixture was stirred 5 h at 80° C. and overnight at 70° C. After addition of further 1.5 eq of potassium carbonate the mixture was stirred 2 h at rt and 2 days at 100° C. The reaction mixture was filtered through a pad of ALOX B and concentrated. The crude was purified by chromatography to give the sub-title compound.

후처리

  1. stirringwas stirred 2 h at rt and 2 days at 100° C
  2. filtrationThe reaction mixture was filtered through a pad of ALOX B
  3. concentrationconcentrated
  4. customThe crude was purified by chromatography

출처 및 근거

ORD 기록
ord-3e3d7d78ce7f47c39764747766e35eeb
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466186B2

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