Potassium Carbonate → HCID 16782287, 화합물

HRID 230792

반응식

HRID 230792 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 16782287HCID 16782287, 화합물수율 40.9%

시약·촉매·용매 1

HCID 19096565Water ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-e616d6cef73c4db7ba90b40ae60674af
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566781B2

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