Ethyl chloroformate → HCID 53727461, 화합물

HRID 651658노트

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HRID 651658 반응식
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]

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 181763372-Iodopyridin-3-amine

생성물 1

HCID 53727461HCID 53727461, 화합물수율 64.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0ca9f03dcb824282a92b3c0d39f9325d
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06281227B1

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