Sodium Dichromate → 2,7-Bis(1-oxo-4-(1-piperidyl)butyl)-9H-fluoren-9-one

HRID 1578653노트

반응식

HRID 1578653 반응식
[N:1]1([CH2:7][CH2:8][CH2:9][C:10]([C:12]2[CH:24]=[CH:23][C:22]3[C:21]4[C:16](=[CH:17][C:18]([C:25](=[O:35])[CH2:26][CH2:27][CH2:28][N:29]5[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]5)=[CH:19][CH:20]=4)[CH2:15][C:14]=3[CH:13]=2)=[O:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=[O:37].[Na+].[Na+]>C(O)(=O)C>[N:1]1([CH2:7][CH2:8][CH2:9][C:10]([C:12]2[CH:24]=[CH:23][C:22]3[C:21]4[C:16](=[CH:17][C:18]([C:25](=[O:35])[CH2:26][CH2:27][CH2:28][N:29]5[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34]5)=[CH:19][CH:20]=4)[C:15](=[O:37])[C:14]=3[CH:13]=2)=[O:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 25408Sodium DichromateHCID 1602411,1'-(9H-Fluorene-2,7-diyl)bis(4-(1-piperidinyl)-1-butanone)

생성물 1

HCID 1475842,7-Bis(1-oxo-4-(1-piperidyl)butyl)-9H-fluoren-9-one

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 9.0 g (0.019 mole) 2,7-bis(4-piperidinobutyryl)fluorene, 7.54 g (0.0253 mole) sodium dichromate and 300 ml of glacial acetic acid is stirred and refluxed for 1 hour. The reaction mixture is evaporated to semi-dryness and made basic using concentrated ammonium hydroxide. The solid which precipitates is filtered, washed with water and chromatographed on alumina using chloroform as the eluant. The solvent is removed from the fraction collected, leaving a solid residue which is recrystallized three times from chloroform-acetone to yield 2,7-bis(4-piperidinobutyryl)fluoren-9-one, M.P. 168°-170°C.

후처리

  1. temperaturerefluxed for 1 hour
  2. customThe reaction mixture is evaporated to semi-dryness
  3. customThe solid which precipitates
  4. filtrationis filtered
  5. washwashed with water
  6. customchromatographed on alumina
  7. customThe solvent is removed from the fraction
  8. customcollected
  9. customleaving a solid residue which
  10. customis recrystallized three times from chloroform-acetone

출처 및 근거

ORD 기록
ord-9ee0872a30df4be8ac37f6f6e29b5190
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03937833

반응 노트

불러오는 중…