Methanesulfonic Acid → HCID 53860911, 화합물

HRID 442870노트

반응식

HRID 442870 반응식
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]

참가 물질

6

반응물 4

HCID 6395Methanesulfonic AcidHCID 274281Diphenylmethyl acetateHCID 516892Sodium BicarbonateHCID 53714353HCID 53714353, 화합물

생성물 1

HCID 53860911HCID 53860911, 화합물수율 69.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ae62ab33e27847428b61b292501bac40
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05891902

반응 노트

불러오는 중…