Potassium Carbonate → HCID 16782287、化合物

HRID 230792

反応式

HRID 230792 の反応式
[SH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([OH:10])=[O:9])=[CH:4][CH:3]=1.Cl.Cl[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C.O>[N:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][S:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([OH:10])=[O:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 23392Picolyl chloride hydrochlorideHCID 957384-Mercaptobenzoic acid

生成物 1

HCID 16782287HCID 16782287、化合物収率 40.9%

試薬・触媒・溶媒 1

HCID 19096565Water ethanol溶媒

実験手順

An ethanol/water mixed solution (2/1, 60 mL) of 4-mercaptobenzenecarboxylic acid (1.0 g), 2-chloromethylpyridine hydrochloride (2.1 g) and potassium carbonate (4.5 g) was heated under reflux for 4 hours. The organic solvent was evaporated off under reduced pressure, and aqueous 5 N hydrochloric acid solution was added to the residue until it became acidic. Water was evaporated off under reduced pressure, and DMF was added to the resulting residue and filtered. The filtrate was concentrated under reduced pressure, and the resulting residue was purified through silica gel column chromatography (chloroform/methanol=9/1 to 4/1) to obtain the entitled compound (650 mg).

後処理

  1. temperatureunder reflux for 4 hours
  2. customThe organic solvent was evaporated off under reduced pressure, and aqueous 5 N hydrochloric acid solution
  3. additionwas added to the residue until it
  4. customWater was evaporated off under reduced pressure, and DMF
  5. additionwas added to the resulting residue
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe resulting residue was purified through silica gel column chromatography (chloroform/methanol=9/1 to 4/1)

出典と根拠

ORDレコード
ord-e616d6cef73c4db7ba90b40ae60674af
出典データセット
uspto-grants-2009_07
特許番号
US07566781B2

関連ノート

読み込み中…