Acetyl chloride → Methyl 2-phenyl-1,3-thiazole-5-carboxylate

HRID 2256810노트

반응식

HRID 2256810 반응식
[C:1](Cl)(=O)C.[C:5]1([C:11]2[S:12][C:13]([C:16]([OH:18])=[O:17])=[CH:14][N:15]=2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>CO>[C:5]1([C:11]2[S:12][C:13]([C:16]([O:18][CH3:1])=[O:17])=[CH:14][N:15]=2)[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1

참가 물질

4

반응물 2

HCID 6367Acetyl chlorideHCID 1390872-Phenyl-5-carboxythiazole

생성물 1

HCID 18913489Methyl 2-phenyl-1,3-thiazole-5-carboxylate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2.5 ml of acetyl chloride were added to a solution of 4.77 g of the acid of Stage B in 160 ml of methanol, and the mixture was refluxed for 18 hours. After evaporating to dryness under reduced pressure, the residue was taken up in ethyl acetate. The mixture was filtered and concentrated to a reduced volume. The crystals were separated off and the mother liquors were washed with sodium hydroxide. Extraction was carried out with ethyl acetate, followed by washing with water and evaporating to dryness. The 2 crystallized fractions were combined to obtain 4.54 g of the desired product melting at 108° C.

후처리

  1. temperaturethe mixture was refluxed for 18 hours
  2. customAfter evaporating to dryness under reduced pressure
  3. filtrationThe mixture was filtered
  4. concentrationconcentrated to a reduced volume
  5. customThe crystals were separated off
  6. washthe mother liquors were washed with sodium hydroxide
  7. extractionExtraction
  8. washby washing with water
  9. customevaporating to dryness

출처 및 근거

ORD 기록
ord-272f3d0548564e16b3427e213d9500ae
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05656607

반응 노트

불러오는 중…