Potassium Carbonate → Methyl 3-(2-chlorothiophenoxymethyl)-thien-2-ylglyoxylate

HRID 1598291ノート

反応式

HRID 1598291 の反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[SH:14].Br[CH2:16][C:17]1[CH:21]=[CH:20][S:19][C:18]=1[C:22](=[O:27])[C:23]([O:25][CH3:26])=[O:24]>CC(C)=O>[Cl:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[S:14][CH2:16][C:17]1[CH:21]=[CH:20][S:19][C:18]=1[C:22](=[O:27])[C:23]([O:25][CH3:26])=[O:24]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 80599o-ChlorothiophenolHCID 21843464Methyl 3-bromomethylthien-2-ylglyoxylate

生成物 1

HCID 131720151Methyl 3-(2-chlorothiophenoxymethyl)-thien-2-ylglyoxylate収率 68.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

2.62 g (19 mmol) of potassium carbonate and 2.74 g (19 mmol) of 2-chlorothiophenol are added to a solution of 5 g (19 mmol) of methyl 3-bromomethylthien-2-ylglyoxylate in 50 ml of acetone, the mixture is stirred for 72 hours at room temperature and filtered and the filtrate is evaporated down. The residue is taken up in methylene chloride, and the solution is washed with Na2CO3 solution, dried and evaporated down. The crude product is recrystallized from methanol. 4.24 g (68%) of the abovementioned compound are obtained.

後処理

  1. filtrationfiltered
  2. customthe filtrate is evaporated down
  3. washthe solution is washed with Na2CO3 solution
  4. customdried
  5. customevaporated down
  6. customThe crude product is recrystallized from methanol

出典と根拠

ORDレコード
ord-2f289c4bf12b41f5a907698d400aa00f
出典データセット
uspto-grants-1998_04
特許番号
US05736566

反応ノート

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