Potassium Carbonate → 1-[1-{4-[5-(4-Amino-1-piperidinyl)pentoyloxy]benzoyl}-4-piperidinyl]-3,4-dihydrocarbostyril

HRID 1708318ノート

反応式

HRID 1708318 の反応式
FC(F)(F)C(NC1CCN(CCCCCO[C:18]2[CH:42]=[CH:41][C:21]([C:22]([N:24]3[CH2:29][CH2:28][CH:27]([N:30]4[C:40]5[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=5)[CH2:34][CH2:33][C:31]4=[O:32])[CH2:26][CH2:25]3)=[O:23])=[CH:20][CH:19]=2)CC1)=O.[C:45](=[O:48])([O-])[O-:46].[K+].[K+]>CO>[NH2:30][CH:27]1[CH2:28][CH2:29][N:24]([CH2:22][CH2:21][CH2:20][CH2:19][C:45]([O:46][C:18]2[CH:42]=[CH:41][C:21]([C:22]([N:24]3[CH2:25][CH2:26][CH:27]([N:30]4[C:40]5[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=5)[CH2:34][CH2:33][C:31]4=[O:32])[CH2:28][CH2:29]3)=[O:23])=[CH:20][CH:19]=2)=[O:48])[CH2:25][CH2:26]1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 189607451-[1-{4-[5-(4-Trifluoroacetylamino-1-piperidinyl)pentyloxy]benzoyl}-4-piperidinyl]-3,4-dihydrocarbostyril

生成物 1

HCID 572403741-[1-{4-[5-(4-Amino-1-piperidinyl)pentoyloxy]benzoyl}-4-piperidinyl]-3,4-dihydrocarbostyril収率 128.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1-[1-{4-[5-(4-Trifluoroacetylamino-1-piperidinyl)pentyloxy]benzoyl}-4-piperidinyl]-3,4-dihydrocarbostyril (1.8 g) is dissolved in methanol (40 ml), and thereto is added potassium carbonate (0.8 g). The mixture is stirred at room temperature overnight. The reaction solution is concentrated and thereto is added water. The mixture is extracted with chloroform, dried over sodium carbonate, and purified by silica gel column chromatography (eluent; dichloromethane:methanol=10:1) to give 1-[1-{4-[5-(4-amino-1-piperidinyl)pentoyloxy]benzoyl}-4-piperidinyl]-3,4-dihydrocarbostyril (1 g) as colorless oil.

後処理

  1. concentrationThe reaction solution is concentrated
  2. additionis added water
  3. extractionThe mixture is extracted with chloroform
  4. dry with materialdried over sodium carbonate
  5. custompurified by silica gel column chromatography (eluent; dichloromethane:methanol=10:1)

出典と根拠

ORDレコード
ord-438adee7253744efbbc261e97762f74d
出典データセット
uspto-grants-1994_10
特許番号
US05356904

反応ノート

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