Ethyl chloroformate → HCID 53727461、化合物

HRID 651658ノート

反応式

HRID 651658 の反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[NH2:7][C:8]1[C:9]([I:14])=[N:10][CH:11]=[CH:12][CH:13]=1>N1C=CC=CC=1>[CH2:5]([O:4][C:2](=[O:3])[NH:7][C:8]1[C:9]([I:14])=[N:10][CH:11]=[CH:12][CH:13]=1)[CH3:6]

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 181763372-Iodopyridin-3-amine

生成物 1

HCID 53727461HCID 53727461、化合物収率 64.6%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
0 °C

実験手順

Ethyl chloroformate (0.91 mL, 9.5 mmol) is added to a solution of 3-amino-2-iodo-pyridine (1.4 g, 6.36 mmol) in 15 mL of pyridine cooled at 0° C. The mixture is stirred at 0° C. for 2 hours and allowed to warm slowly to room temperature. At this time, excess pyridine is removed in vacuo. The residue is diluted with EtOAc and washed with water, 1N HCl and saturated NaHCO3. The organic layer is dried over MgSO4, filtered and concentrated in vacuo. The crude product is purified by column chromatography eluting with 30% EtOAc/hexanes to give the title compound (1.2 g, 4.11 mmol) as a beige solid.

後処理

  1. temperatureto warm slowly to room temperature
  2. customAt this time, excess pyridine is removed in vacuo
  3. additionThe residue is diluted with EtOAc
  4. washwashed with water, 1N HCl and saturated NaHCO3
  5. dry with materialThe organic layer is dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe crude product is purified by column chromatography
  9. washeluting with 30% EtOAc/hexanes

出典と根拠

ORDレコード
ord-0ca9f03dcb824282a92b3c0d39f9325d
出典データセット
uspto-grants-2001_08
特許番号
US06281227B1

反応ノート

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