Potassium Carbonate → HCID 21288084、化合物

HRID 868212ノート

反応式

HRID 868212 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 21288084HCID 21288084、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-173754239b17438095e56780c90626e7
出典データセット
uspto-grants-1988_10
特許番号
US04778803

反応ノート

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