Methanesulfonic Acid → HCID 15858911、化合物

HRID 442858ノート

反応式

HRID 442858 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.[Cl:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[N:25]1[CH2:30][CH2:29][N:28]([C:31]([C:33]2[NH:34][C:35]3[C:40]([CH:41]=2)=[CH:39][CH:38]=[CH:37][CH:36]=3)=[O:32])[CH2:27][CH2:26]1.CS(O)(=O)=O.C(=O)(O)[O-].[Na+]>C(Cl)Cl.C(Cl)(Cl)Cl>[Cl:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[N:25]1[CH2:30][CH2:29][N:28]([C:31]([C:33]2[NH:34][C:35]3[C:40]([C:41]=2[CH:5]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[CH:39][CH:38]=[CH:37][CH:36]=3)=[O:32])[CH2:27][CH2:26]1

参加物

7

反応物 4

HCID 6395Methanesulfonic AcidHCID 274281Diphenylmethyl acetateHCID 516892Sodium BicarbonateHCID 17877334HCID 17877334、化合物

生成物 1

HCID 15858911HCID 15858911、化合物収率 89.5%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

Benzhydryl acetate (2.2 g, 9.71 mmol) and 2-[4-(2-chlorophenyl)piperazinylcarbonyl]indole (3.0 g, 8.83 mmol) were dissolved in a mixed solvent of methylene chloride (50 ml) and chloroform (50 ml), and methanesulfonic acid (1.72 ml, 26.5 mmol) was added thereto, followed by stirring at room temperature for 3 hours. 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 6.5 g of a crude product. The obtained crude product was washed with ethanol (60 ml) under heating to give 4.0 g (yield: 89%) of the title compound.

後処理

  1. additionwas added
  2. extractionfollowed by extraction with chloroform
  3. washThe resulting organic layer was washed with a saturated aqueous solution of sodium bicarbonate
  4. dry with materiala saturated aqueous solution of sodium chloride, and dried over magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customto give 6.5 g of a crude product
  7. customThe obtained crude product
  8. washwas washed with ethanol (60 ml)
  9. temperatureunder heating

出典と根拠

ORDレコード
ord-657c9ab476994acc9cbf9d24577af1e2
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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