Methanesulfonic Acid → HCID 53860911、化合物

HRID 442870ノート

反応式

HRID 442870 の反応式
C(O[CH:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)(=O)C.[CH2:18]([N:20]([CH2:33][CH3:34])[S:21]([C:24]1[NH:25][C:26]2[C:31]([CH:32]=1)=[CH:30][CH:29]=[CH:28][CH:27]=2)(=[O:23])=[O:22])[CH3:19].CS(O)(=O)=O.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH2:33]([N:20]([CH2:18][CH3:19])[S:21]([C:24]1[NH:25][C:26]2[C:31]([C:32]=1[CH:5]([C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)=[CH:30][CH:29]=[CH:28][CH:27]=2)(=[O:22])=[O:23])[CH3:34]

参加物

6

反応物 4

HCID 6395Methanesulfonic AcidHCID 274281Diphenylmethyl acetateHCID 516892Sodium BicarbonateHCID 53714353HCID 53714353、化合物

生成物 1

HCID 53860911HCID 53860911、化合物収率 69.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of benzhydryl acetate (0.77 g, 3.39 mmol) and N,N-diethylindole-2-sulfonamide (0.9 g, 3.39 mmol) in 20 ml of methylene chloride was added methanesulfonic acid (0.7 ml, 10.7 mmol), followed by stirring at room temperature for one hour. A saturated aqueous solution of sodium bicarbonate was added to the reaction solution for neutralization followed by extraction with chloroform. The resulting organic layer was washed with a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure to give a crude product. The obtained crude product was crystallized from diisopropyl ether to give 0.99 g (yield: 67%) of the title compound.

後処理

  1. extractionfollowed by extraction with chloroform
  2. washThe resulting organic layer was washed with a saturated aqueous solution of sodium bicarbonate
  3. dry with materiala saturated aqueous solution of sodium chloride, and dried over magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customto give a crude product
  6. customThe obtained crude product
  7. customwas crystallized from diisopropyl ether

出典と根拠

ORDレコード
ord-ae62ab33e27847428b61b292501bac40
出典データセット
uspto-grants-1999_04
特許番号
US05891902

反応ノート

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