Ethyl Acetate → 5-Nitro-2-(1-pyrrolidinyl)pyridine

HRID 496286

반응식

HRID 496286 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].[NH:17]1[CH2:21][CH2:20][CH2:19][CH2:18]1.CCOC(C)=O>CN(C=O)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([N:17]2[CH2:21][CH2:20][CH2:19][CH2:18]2)=[N:3][CH:4]=1)([O-:10])=[O:9]

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 31268PyrrolidineHCID 783082-Chloro-5-nitropyridine

생성물 1

HCID 3168235-Nitro-2-(1-pyrrolidinyl)pyridine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirring mixture of 2-chloro-5-nitropyridine (5.0 g, 31.5 mmol), potassium carbonate (7.0 g, 50.4 mmol), in 65 ml of DMF add pyrrolidine (6.7 g, 95 mmol) and stir at room temperature for 72 h. Dilute reaction mixture with 100 ml EtOAc and wash 2 times with 100 ml saturated NaHCO3, and 2 times with 100 ml of brine. Dry organics over Na2SO4, and evaporate in vacuo to obtain 5-nitro-2-pyrrolidin-1-yl-pyridine. Mass spec.: m+1=194 (AP+). B. 6-Pyrrolidin-1-yl-pyridin-3-ylamine

후처리

  1. additionDilute
  2. washwash 2 times with 100 ml saturated NaHCO3, and 2 times with 100 ml of brine
  3. customDry organics over Na2SO4, and evaporate in vacuo

출처 및 근거

ORD 기록
ord-5c7010abf7794b8eba450c893c6f2590
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06943199B2

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