Methanol → HCID 67509641、化合物

HRID 623449ノート

反応式

HRID 623449 の反応式
[Cl:1][C:2]1[C:3]([O:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].S(=O)(=O)(O)O.[CH3:22]O>>[Cl:1][C:2]1[C:3]([O:11][CH2:12][C:13]([F:15])([F:16])[F:14])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7]([O:9][CH3:22])=[O:8]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 167824855-Chloro-6-(2,2,2-trifluoroethoxy)pyridine-3-carboxylic acid

生成物 1

HCID 67509641HCID 67509641、化合物収率 56%

実験手順

A mixture of 5-chloro-6-(2,2,2-trifluoroethoxy)nicotinic acid (5.6 g, 21.9 mmol, Step-1 of Amine-5) and sulfuric acid (0.12 mL, 2.25 mmol) in methanol (40 mL) is refluxed with stirring for 2 days. After removal of the solvent, the residue is poured into 2M sodium hydroxide (100 mL) and extracted with ethyl acetate and dried over sodium sulfate and concentrated in vacuo to give 3.28 g (56% yield) of the title compound as a white solid.

後処理

  1. temperatureis refluxed
  2. customAfter removal of the solvent
  3. additionthe residue is poured into 2M sodium hydroxide (100 mL)
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-de33234e42ce4e25a6fa438ffcd03b7b
出典データセット
uspto-grants-2016_04
特許番号
US09302991B2

反応ノート

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