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

HRID 341477ノート

反応式

HRID 341477 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-d3be77bdd860451bb68698dc436494ad
出典データセット
uspto-grants-2014_11
特許番号
US08895733B2

反応ノート

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