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

HRID 496286

反応式

HRID 496286 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-5c7010abf7794b8eba450c893c6f2590
出典データセット
uspto-grants-2005_09
特許番号
US06943199B2

関連ノート

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