Ethyl Acetate → HCID 54318896, 화합물

HRID 22413

반응식

HRID 22413 반응식
[C:1]1([S:7]([NH:10][C:11]([C:13]2[CH:14]=[CH:15][C:16]([C:19]([O-:21])=[O:20])=[N:17][CH:18]=2)=[O:12])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(OCC)(=O)C.[CH3:28][CH2:29][CH:30](O)[CH2:31][CH3:32]>S(=O)(=O)(O)O>[C:1]1([S:7]([NH:10][C:11]([C:13]2[CH:14]=[CH:15][C:16]([C:19]([O:21][CH:30]([CH2:31][CH3:32])[CH2:29][CH3:28])=[O:20])=[N:17][CH:18]=2)=[O:12])(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 114283-PentanolHCID 199281735-[((Phenylsulfonyl)amino)carbonyl]-pyridine-2-carboxylate

생성물 1

HCID 54318896HCID 54318896, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

반응 조건

온도
90 °C

실험 절차

5 drops of concentrated sulfuric acid were added to 0.9 g (2.94 mmol) of 5-[((phenylsulfonyl)amino)carbonyl]-pyridine-2-carboxylate in 30 ml of 3-pentanol, while stirring, and the mixture was heated at 90° C. for 6 hours. The excess 3-pentanol was distilled off in vacuo and the residue was treated with ethyl acetate. The crystalline crude product was combined with the product obtained from the mother liquor by purification by column chromatography (melting point 186° to 187° C.), treated with hot ethyl acetate, cooled, filtered off with suction and washed with ethyl acetate. This gave 0.55 g of the colorless title compound, melting point 182° to 183° C.

후처리

  1. distillationThe excess 3-pentanol was distilled off in vacuo
  2. additionthe residue was treated with ethyl acetate
  3. customobtained from the mother liquor by purification by column chromatography (melting point 186° to 187° C.)
  4. temperaturecooled
  5. filtrationfiltered off with suction
  6. washwashed with ethyl acetate

출처 및 근거

ORD 기록
ord-6bd2cbbffc724748a70641fce04391fe
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05428046

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