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Potassium Iodide → 5-(1-piperidyl)-1-[7-[5-(1-piperidyl)pentanoyl]-9H-xanthen-2-yl]pentan-1-one

HRID 1076911
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HRID 1076911 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[O:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26]Cl)=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7].[I-].[K+].[NH:31]1[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1>O1CCCC1>[N:31]1([CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]2[CH:21]=[CH:20][C:19]3[O:18][C:17]4[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26][N:31]5[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]5)=[CH:15][CH:16]=4)[CH2:11][C:10]=3[CH:9]=2)=[O:7])[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1
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참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 8082PiperidineHCID 123402842,7-Bis(5-chlorovaleryl)-xanthene

생성물 1

HCID 5154035-(1-piperidyl)-1-[7-[5-(1-piperidyl)pentanoyl]-9H-xanthen-2-yl]pentan-1-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
100 °C

실험 절차

A mixture of 30 g. (0.07 mole) of 2,7-bis(5-chlorovaleryl)-xanthene, 2 g of potassium iodide, 100 ml. of piperidine, and 200 ml. of tetrahydrofuran was heated and stirred at 100°C. for 24 hours. After cooling, the tetrahydrofuran was evaporated off and the resulting mixture was poured into water. The resulting solid was filtered off and recrystallized twice from heptane to give the desired product after drying at 80°C. under vacuum. M.P. 129°-130°C.

후처리

  1. additionA mixture of 30 g
  2. temperatureAfter cooling
  3. customthe tetrahydrofuran was evaporated off
  4. additionthe resulting mixture was poured into water
  5. filtrationThe resulting solid was filtered off
  6. customrecrystallized twice from heptane

출처 및 근거

ORD 기록
ord-6c5a6223dbc0454eaa870725c351cf93
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03957989

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