Sodium Bicarbonate → N-{1-[p-(5-Isoquinolinesulfonyloxy)benzyl]-2-(4-oxopiperidino)ethyl)-N-methyl-5-isoquinolinesulfonamide

HRID 1090568

반응식

HRID 1090568 반응식
C1CO[C:3]2([CH2:8][CH2:7][N:6]([CH2:9][CH:10]([N:32]([CH3:46])[S:33]([C:36]3[C:37]4[CH:38]=[CH:39][N:40]=[CH:41][C:42]=4[CH:43]=[CH:44][CH:45]=3)(=[O:35])=[O:34])[CH2:11][C:12]3[CH:17]=[CH:16][C:15]([O:18][S:19]([C:22]4[C:23]5[CH:24]=[CH:25][N:26]=[CH:27][C:28]=5[CH:29]=[CH:30][CH:31]=4)(=[O:21])=[O:20])=[CH:14][CH:13]=3)[CH2:5][CH2:4]2)[O:2]1.C(=O)(O)[O-].[Na+]>Cl>[CH:27]1[C:28]2[CH:29]=[CH:30][CH:31]=[C:22]([S:19]([O:18][C:15]3[CH:14]=[CH:13][C:12]([CH2:11][CH:10]([N:32]([CH3:46])[S:33]([C:36]4[C:37]5[CH:38]=[CH:39][N:40]=[CH:41][C:42]=5[CH:43]=[CH:44][CH:45]=4)(=[O:34])=[O:35])[CH2:9][N:6]4[CH2:7][CH2:8][C:3](=[O:2])[CH2:4][CH2:5]4)=[CH:17][CH:16]=3)(=[O:20])=[O:21])[C:23]=2[CH:24]=[CH:25][N:26]=1

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 53669357N-{2-(4,4-ethylenedioxypiperidino)-1-[p-(5-isoquinolinesulfonyloxy)benzyl]ethyl}-N-methyl-5-isoquinolinesulfonamide

생성물 1

HCID 19796283N-{1-[p-(5-Isoquinolinesulfonyloxy)benzyl]-2-(4-oxopiperidino)ethyl)-N-methyl-5-isoquinolinesulfonamide수율 92.3%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

2.57 g of the product of Example 94 was dissolved in 50 ml of 3 N hydrochloric acid, and after refluxing for 6 hours and then cooling, the reaction mixture was alkalized with saturated sodium bicarbonate aqueous solution and extracted twice with 200 ml of chloroform. The extract was dried over magnesium sulfate and evaporated under a reduced pressure to remove the solvent, and resulting residue was applied to a silica gel column and eluted with chloroform/methanol (50:1) to obtain 2.22 g of the title compound in a colorless amorphous form.

후처리

  1. temperatureafter refluxing for 6 hours
  2. temperaturecooling
  3. extractionextracted twice with 200 ml of chloroform
  4. dry with materialThe extract was dried over magnesium sulfate
  5. customevaporated under a reduced pressure
  6. customto remove the solvent
  7. customresulting residue
  8. washeluted with chloroform/methanol (50:1)

출처 및 근거

ORD 기록
ord-6fa053d3be124172b1d16d31771d68f5
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05081246

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