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

HRID 34999노트

반응식

HRID 34999 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c363dc78aa294123a31bd51bae97f9b1
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764617

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