Methanol → HCID 67509641, 화합물

HRID 623449노트

반응식

HRID 623449 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

HCID 67509641HCID 67509641, 화합물수율 56%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-de33234e42ce4e25a6fa438ffcd03b7b
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302991B2

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