Fumaric Acid → N-(1-Phenyl-3-piperidinopropyl)quinaldinamide fumarate

HRID 34999ノート

反応式

HRID 34999 の反応式
[C:1]1([CH:7]([NH:16][C:17]([CH2:19][C:20]2[CH:29]=[CH:28][C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[N:21]=2)=[O:18])[CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:30]([OH:37])(=[O:36])/[CH:31]=[CH:32]/[C:33]([OH:35])=[O:34]>C(O)C.CC(C)=O>[C:30]([OH:37])(=[O:36])/[CH:31]=[CH:32]/[C:33]([OH:35])=[O:34].[C:1]1([CH:7]([NH:16][C:17]([CH2:19][C:20]2[CH:29]=[CH:28][C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[N:21]=2)=[O:18])[CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 2

HCID 444972Fumaric AcidHCID 67930081N-(1-phenyl-3-piperidinopropyl)quinaldinamide

生成物 1

HCID 86742335N-(1-Phenyl-3-piperidinopropyl)quinaldinamide fumarate収率 78%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 702Ethanol溶媒2 回

実験手順

To a solution of 3.02 g (8.1 mmol.) of N-(1-phenyl-3-piperidinopropyl)quinaldinamide in a mixture of 18 ml of ethanol and 8 ml of acetone was added a solution of 0.939 g (8.1 mmol.) of fumaric acid in 20 ml of hot ethanol. The resulting mixture was stirred at room temperature and subsequently under chilling with ice. Precipitated crystals were collected by filtration and washed with acetone. The washed crystals were suspended in 60 ml of n-hexane and the suspension was refluxed for 1.5 hours. The crystals were collected by filtration, washed with n-hexane and dried. Thus, 3.10 g (yield: 78%) of the subject compound was obtained as a white crystalline product.

後処理

  1. temperaturesubsequently under chilling with ice
  2. customPrecipitated crystals
  3. filtrationwere collected by filtration
  4. washwashed with acetone
  5. temperaturethe suspension was refluxed for 1.5 hours
  6. filtrationThe crystals were collected by filtration
  7. washwashed with n-hexane
  8. customdried

出典と根拠

ORDレコード
ord-c363dc78aa294123a31bd51bae97f9b1
出典データセット
uspto-grants-1988_08
特許番号
US04764617

反応ノート

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