Oxalyl chloride → 3-Pyridinecarbonyl chloride, 6-(2,2,2-trifluoroethoxy)-

HRID 341477노트

반응식

HRID 341477 반응식
[F:1][C:2]([F:15])([F:14])[CH2:3][O:4][C:5]1[CH:13]=[CH:12][C:8]([C:9](O)=[O:10])=[CH:7][N:6]=1.C(Cl)(=O)C([Cl:19])=O>ClCCCl>[F:1][C:2]([F:15])([F:14])[CH2:3][O:4][C:5]1[CH:13]=[CH:12][C:8]([C:9]([Cl:19])=[O:10])=[CH:7][N:6]=1

참가 물질

4

반응물 2

HCID 65578Oxalyl chlorideHCID 27810286-(2,2,2-Trifluoroethoxy)pyridine-3-carboxylic acid

생성물 1

HCID 235127223-Pyridinecarbonyl chloride, 6-(2,2,2-trifluoroethoxy)-수율 102%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

To 6-(2,2,2-trifluoro-ethoxy)-nicotinic acid (100 mg, 0.45 mmol) was added DCE (5 mL) and oxalyl chloride (60 ul, 0.68 mmol) under an atmosphere of nitrogen. The mixture was stirred at rt for 1.5 h then heated at 80 C for 2 h and after cooling to room temperature, evaporated to give the title compound as a pale yellow oil (110 mg, 100%). Method C HPLC-MS (in MeOH, identifying the methyl ester): MH+ requires m/z=236. Found: m/z=236, Rt=1.41 min (95%).

후처리

  1. temperaturethen heated at 80 C for 2 h
  2. temperatureafter cooling to room temperature
  3. customevaporated

출처 및 근거

ORD 기록
ord-d3be77bdd860451bb68698dc436494ad
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895733B2

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