Ethyl Thioglycolate → Ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate

HRID 9638

반응식

HRID 9638 반응식
[H-].[Na+].F[P-](F)(F)(F)(F)F.Cl[C:11]([C:18]1[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][CH:19]=1)=[CH:12][C:13](=[N+](C)C)[CH3:14].[C:28]([O:32][CH2:33][CH3:34])(=[O:31])[CH2:29][SH:30]>C(O)C>[CH3:14][C:13]1[CH:12]=[C:11]([C:18]2[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][CH:19]=2)[S:30][C:29]=1[C:28]([O:32][CH2:33][CH3:34])=[O:31]

참가 물질

5

반응물 3

HCID 12185Ethyl ThioglycolateHCID 24758Sodium hydrideHCID 86593913N-{3-chloro-1-methyl-3-[4-(trifluoromethyl)phenyl]prop-2-enylidene}-N-methylmethanaminium hexafluorophosphate2회

생성물 1

HCID 15946279Ethyl 3-methyl-5-[4-(trifluoromethyl)phenyl]thiophene-2-carboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
110 °C

실험 절차

Sodium hydride (60% dispersion in mineral oil, 0.528 g) was added to dry ethanol (20 ml), N-{3-chloro-1-methyl-3-[4-(trifluoromethyl)phenyl]prop-2-enylidene}-N-methylmethanaminium hexafluorophosphate (intermediate 34, 2.8 g) was added followed by ethyl thioglycolate (0.79 g) and the mixture heated at 110° C. for 2 hours under nitrogen. The cooled mixture was concentrated in vacuo and the residue partitioned between water and diethyl ether. The organic layer was collected, dried over magnesium sulphate and concentrated to give the title compound as a brown solid.

후처리

  1. additionwas added
  2. concentrationThe cooled mixture was concentrated in vacuo
  3. customthe residue partitioned between water and diethyl ether
  4. customThe organic layer was collected
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-6ea3ca517d7342f6ac2c54fa506a38d2
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091237B2

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