2,3,4-Trimethoxybenzaldehyde → 2-[4-(2,3,4-Trimethoxybenzyl)-1-piperazinyl]-5-n-propylbenzenesulfonic acid

HRID 344665노트

반응식

HRID 344665 반응식
C([BH3-])#N.[Na+].[N:5]1([C:11]2[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH3:19])=[CH:13][C:12]=2[S:20]([OH:23])(=[O:22])=[O:21])[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1.[CH3:24][O:25][C:26]1[C:33]([O:34][CH3:35])=[C:32]([O:36][CH3:37])[CH:31]=[CH:30][C:27]=1[CH:28]=O>CO.[Cl-].[Zn+2].[Cl-]>[CH3:24][O:25][C:26]1[C:33]([O:34][CH3:35])=[C:32]([O:36][CH3:37])[CH:31]=[CH:30][C:27]=1[CH2:28][N:8]1[CH2:9][CH2:10][N:5]([C:11]2[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH3:19])=[CH:13][C:12]=2[S:20]([OH:23])(=[O:21])=[O:22])[CH2:6][CH2:7]1

참가 물질

6

반응물 3

HCID 750062,3,4-TrimethoxybenzaldehydeHCID 30273132-(1-Piperazinyl)-5-n-propylbenzenesulfonic acidHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 103222122-[4-(2,3,4-Trimethoxybenzyl)-1-piperazinyl]-5-n-propylbenzenesulfonic acid수율 59.7%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 887Methanol용매

실험 절차

Into a solution of 0.10 g of sodium cyanoborohydride dissolved in 2 ml of a methanol solution was added 0.10 g of zinc chloride, and the mixture was stirred for 5 minutes. Then, 0.40 g of 2-(1-piperazinyl)-5-n-propylbenzenesulfonic acid and 0.58 g of 2,3,4-trimethoxybenzaldehyde were added to carry out the reaction at room temperature for 2 hours. The organic layer was extracted by addition of an aqueous sodium chloride and tetrahydrofuran, and after evaporation of tetrahydrofuran under reduced pressure from the extract, the residue was purified by silicagel column chromatography (eluant:chloroform: methanol:acetic acid=500:100:6) to give 0.39 g (yield: 58.5%) of the above title product as a glassy solid.

후처리

  1. customthe reaction at room temperature for 2 hours
  2. extractionThe organic layer was extracted by addition of an aqueous sodium chloride and tetrahydrofuran
  3. customafter evaporation of tetrahydrofuran under reduced pressure from the extract
  4. customthe residue was purified by silicagel column chromatography (eluant:chloroform: methanol:acetic acid=500:100:6)

출처 및 근거

ORD 기록
ord-f712bf46adec498eb2049a7584260849
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05053409

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