Potassium Carbonate → HCID 21288084, 화합물

HRID 868212노트

반응식

HRID 868212 반응식
[OH:1][C:2]1[CH:3]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=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+]>CC(=O)CC>[N:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][O:1][C:2]1[CH:3]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 23392Picolyl chloride hydrochlorideHCID 13277908Methyl 4-hydroxythiophene-2-carboxylate

생성물 1

HCID 21288084HCID 21288084, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

3.00 g (19.0 mmol) of methyl 4-hydroxy-2-thiophenecarboxylate, 3.11 g (19.0 mmol) of 2-chloromethylpyridine hydrochloride and 5.24 g (37.9 mmol) of potassium carbonate are heated under reflux in 60 ml of absolute 2-butanone for 10 hours under nitrogen. The mixture is then evaporated in vacuo and the residue is partitioned between methylene chloride and saturated sodium bicarbonate solution. The aqueous phase is extracted twice more with 100 ml of methylene chloride each time and the combined organic phases are dried over sodium sulfate/active charcoal, filtered and evaporated. The residue is digested with diisopropyl ether.

후처리

  1. customThe mixture is then evaporated in vacuo
  2. customthe residue is partitioned between methylene chloride and saturated sodium bicarbonate solution
  3. extractionThe aqueous phase is extracted twice more with 100 ml of methylene chloride each time
  4. dry with materialthe combined organic phases are dried over sodium sulfate/active charcoal
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-173754239b17438095e56780c90626e7
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04778803

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