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

HRID 1379708노트

반응식

HRID 1379708 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1aa17da1ce18495e98ba69d5152763d2
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05672616

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