Hydrochloric Acid → 6-(Methylthio)nicotinic acid

HRID 2365248

反応式

HRID 2365248 の反応式
F[C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1.[CH3:11][S-:12].[Na+].Cl>CS(C)=O.C(OCC)(=O)C>[CH3:11][S:12][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][N:3]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 2428196-Fluoronicotinic AcidHCID 4378561Sodium methanethiolate

生成物 1

HCID 8194096-(Methylthio)nicotinic acid

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

To a solution of 6-fluoronicotinic acid (0.995 g, 7.05 mmol) in 14 mL of dimethylsulfoxide was added sodium thiomethoxide (1.24 g, 17.6 mmol). The mixture was heated 80° C. for 1 hr, cooled to ambient temperature, and treated with concentrated hydrochloric acid (4.5 mL, 0.054 mol). After 15 min, the mixture was diluted with ethyl acetate and concentrated in vacuo to provide 6-(methylthio)nicotinic acid that gave a mass ion (ES+) of 170.1 for [M+H]+.

後処理

  1. temperaturecooled to ambient temperature
  2. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-d54c21f2e82f47e0a7aa21e15eecfe8c
出典データセット
uspto-grants-2014_04
特許番号
US08697690B2

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