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

HRID 1090568

反応式

HRID 1090568 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-6fa053d3be124172b1d16d31771d68f5
出典データセット
uspto-grants-1992_01
特許番号
US05081246

関連ノート

読み込み中…