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

HRID 1074392ノート

反応式

HRID 1074392 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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##

後処理

  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

出典と根拠

ORDレコード
ord-d33de4cc8e604d8ea697708b4ad14219
出典データセット
uspto-grants-1983_07
特許番号
US04391807

反応ノート

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