Potassium Carbonate → HCID 21271267、化合物

HRID 1194008ノート

反応式

HRID 1194008 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.I[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]1[O:23][N:22]=[C:21]([CH3:24])[CH:20]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:24][C:21]1[CH:20]=[C:19]([CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][O:1][C:2]2[CH:3]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=2)[O:23][N:22]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 13277908Methyl 4-hydroxythiophene-2-carboxylateHCID 21271268HCID 21271268、化合物

生成物 1

HCID 21271267HCID 21271267、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

6.42 g (40.60 mmol) of methyl 4-hydroxy-2-thiophenecarboxylate (XIa) and 11.88 g (38.67 mmol) of 5-(7-iodoheptyl)-3-methyl-isoxazole (IX) are heated under reflux with 5.34 g (40.60 mmol) of potassium carbonate (K2CO3) in 130 ml of anhydrous acetone for 8 hours. After the mixture has been left to stand overnight, it is concentrated, the residue is partitioned between 2N NaOH and ether and the aqueous phase is extracted several times with a total of 150 ml of ether. The organic phase is dried over sodium sulfate/active charcoal and evaporated.

後処理

  1. waitAfter the mixture has been left
  2. concentrationit is concentrated
  3. customthe residue is partitioned between 2N NaOH and ether
  4. extractionthe aqueous phase is extracted several times with a total of 150 ml of ether
  5. dry with materialThe organic phase is dried over sodium sulfate/active charcoal
  6. customevaporated

出典と根拠

ORDレコード
ord-d1919189db3f431594790d2f33c6fc7a
出典データセット
uspto-grants-1989_03
特許番号
US04812472

反応ノート

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