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Fumaric Acid → N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide fumarate

HRID 565754
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HRID 565754 반응식
[CH:1]1([NH:4][S:5]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][N:17]([CH:20]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[CH:28]=3)[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:16][CH2:15]2)(=[O:7])=[O:6])[CH2:3][CH2:2]1.[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38]>C(O)C>[C:34]([OH:41])(=[O:40])/[CH:35]=[CH:36]/[C:37]([OH:39])=[O:38].[CH:1]1([NH:4][S:5]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][N:17]([CH:20]([C:27]3[CH:32]=[CH:31][CH:30]=[C:29]([Cl:33])[CH:28]=3)[C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:16][CH2:15]2)(=[O:7])=[O:6])[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 444972Fumaric AcidHCID 15895709N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide

생성물 1

HCID 22111604N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide fumarate수율 93.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

N-Cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide (13.03 g, 26.59 mmol) prepared in the same manner as in Example 1 was dissolved in ethanol (100 ml). Fumaric acid (4.01 g, 34.55 mmol) was added thereto. After dissolving the mixture with heating, the mixture was cooled in an ice bath to allow the mixture to crystallize. The crystals were filtered, washed with a small amount of ethanol, and dried at 80° C. in vacuo, to give N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide fumarate (15.11 g) as colorless prisms (yield based on N-cyclopropyl-6-[4-[(3-chlorophenyl)phenylmethyl]-1-piperazinyl]hexanesulfonamide: 93.7%).

후처리

  1. dissolutionAfter dissolving the mixture
  2. temperaturewith heating
  3. temperaturethe mixture was cooled in an ice bath
  4. customto crystallize
  5. filtrationThe crystals were filtered
  6. washwashed with a small amount of ethanol
  7. customdried at 80° C. in vacuo
  8. customto give

출처 및 근거

ORD 기록
ord-81a4245d6a364764a3d2449a5162e2e5
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06172228B2

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