Potassium Carbonate → 2,2-Dimethyl-5-[(4-phenyl-thiophen-2-ylamino)-methylene]-[1,3]dioxane-4,6-dione

HRID 215988노트

반응식

HRID 215988 반응식
[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[CH2:6][C:4](=[O:5])[O:3]1.[CH:11](OCC)(OCC)OCC.[C:21]1([C:27]2[CH:28]=[C:29]([NH2:32])[S:30][CH:31]=2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl>[CH3:1][C:2]1([CH3:10])[O:9][C:7](=[O:8])[C:6](=[CH:11][NH:32][C:29]2[S:30][CH:31]=[C:27]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:28]=2)[C:4](=[O:5])[O:3]1

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 31214Ethyl orthoformateHCID 125259964-Phenylthiophen-2-amine

생성물 1

HCID 684322042,2-Dimethyl-5-[(4-phenyl-thiophen-2-ylamino)-methylene]-[1,3]dioxane-4,6-dione

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
30 °C

실험 절차

Meldrum's acid (1.05 g, 7.3 mmol) was added to triethyl orthoformate (50 ml) and stirred at 30° C. for 1 hr. The reaction mixture was cooled to room temperature and 4-phenyl-thiophene-2-yl-amine (1.07 g, 6.1 mmol) was added in portions. The reaction mixture was heated to 85° C. and stirred at this temperature overnight before cooling to room temperature. The solvent was removed in vacuo to give a residue which was dissolved in DCM and treated with potassium carbonate. After stirring for 30 min the mixture was filtered and the solvent removed in vacuo to give 2,2-dimethyl-5-[(4-phenyl-thiophen-2-ylamino)-methylene]-[1,3]dioxane-4,6-dione. Yield=1.41 g (70%).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. temperatureThe reaction mixture was heated to 85° C.
  3. stirringstirred at this temperature overnight
  4. temperaturebefore cooling to room temperature
  5. customThe solvent was removed in vacuo
  6. customto give a residue which
  7. stirringAfter stirring for 30 min the mixture
  8. filtrationwas filtered
  9. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-80bd03ecdfb34b3fb2ce77202ce2340f
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08193215B2

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