Acetone → 6-(1-Piperidinyl)-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine

HRID 1074392노트

반응식

HRID 1074392 반응식
Cl[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][CH:13]=[CH:14][N:4]2[N:3]=1.[NH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1.CC(C)=O>C(Cl)Cl>[N:15]1([C:2]2[C:11]3[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=3[C:5]3=[N:12][CH:13]=[CH:14][N:4]3[N:3]=2)[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1

참가 물질

5

반응물 3

HCID 180AcetoneHCID 8082PiperidineHCID 131789756-Chloro-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine

생성물 1

HCID 131789776-(1-Piperidinyl)-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture was prepared by adding 15 g of 6-chloro-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine to 30.5 g of piperidine and the mixture was heated at reflux for 72 hours. The mixture was subjected to preparative liquid chromatography using 15% acetone in methylene chloride to separate the desired product from the impurities. The appropriate fractions from the chromatography were combined and the solvent was evaporated under reduced pressure. The resulting solid was collected by filtration and dried to give 6-(1-piperidinyl)-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine melting at about 95° C. This compound has the following structural formula ##STR2##

후처리

  1. customA mixture was prepared
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 72 hours
  4. customto separate the desired product from the impurities
  5. customthe solvent was evaporated under reduced pressure
  6. filtrationThe resulting solid was collected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-d33de4cc8e604d8ea697708b4ad14219
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04391807

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