Ethyl Acetate → HCID 54318896、化合物

HRID 22413

反応式

HRID 22413 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 54318896HCID 54318896、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6bd2cbbffc724748a70641fce04391fe
出典データセット
uspto-grants-1995_06
特許番号
US05428046

関連ノート

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