Sodium Bicarbonate → 1-{3-{Bis[4-(methoxymethoxy)phenyl]methyl}indol-2-ylcarbonyl}-4-(2-chlorophenyl)piperazine

HRID 442848ノート

反応式

HRID 442848 の反応式
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:22]=[CH:21][C:8]([CH:9](O)[C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:17][O:18][CH3:19])=[CH:12][CH:11]=2)=[CH:7][CH:6]=1.[Cl:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=1[N:30]1[CH2:35][CH2:34][N:33]([C:36]([C:38]2[NH:39][C:40]3[C:45]([CH:46]=2)=[CH:44][CH:43]=[CH:42][CH:41]=3)=[O:37])[CH2:32][CH2:31]1.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:22]=[CH:21][C:8]([CH:9]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:17][O:18][CH3:19])=[CH:12][CH:11]=2)[C:46]2[C:45]3[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=3)[NH:39][C:38]=2[C:36]([N:33]2[CH2:32][CH2:31][N:30]([C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=3[Cl:23])[CH2:35][CH2:34]2)=[O:37])=[CH:7][CH:6]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 17877334HCID 17877334、化合物HCID 54082355HCID 54082355、化合物

生成物 1

HCID 158589011-{3-{Bis[4-(methoxymethoxy)phenyl]methyl}indol-2-ylcarbonyl}-4-(2-chlorophenyl)piperazine収率 82%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Boron trifluoride-ether complex (0.36 ml, 2.94 mmol) was added dropwise at 0° C. to a solution of 4,4'-bis(methoxymethoxy)benzhydrol (8.96 g, 29.43 mmol) and 1-(2-chlorophenyl)-4-(indol-2-ylcarbonyl)piperazine (10.0 g, 29.43 mmol) in 200 ml of methylene chloride, followed by stirring at 0° C. to room temperature for 2 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 a crude product. The obtained crude product was recrystallized from ethanol to, give 15.1 g (yield: 82%) 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 recrystallized from ethanol to,

出典と根拠

ORDレコード
ord-6a035043ba434d559b4d4ca58b09138a
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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