Hydrochloric Acid → HCID 11460950, 화합물

HRID 488980

반응식

HRID 488980 반응식
CC(CC)[O-].CC(CC)[O-].CC(CC)[O-].[Al+3].C1(O)CCCCC1.[CH3:24][C:25]1[CH:26]=[CH:27][C:28]2[CH:29]=[C:30]3[C:43]([C:44](=O)[C:45]=2[CH:46]=1)=[CH:42][C:41]1[C:32]([C:33](=O)[C:34]2[C:39]([CH:40]=1)=[CH:38][CH:37]=[C:36]([CH3:48])[CH:35]=2)=[CH:31]3.Cl>C1COCC1.CC(C)=O>[CH3:24][C:25]1[CH:26]=[CH:27][C:28]2[C:45](=[CH:44][C:43]3[C:30]([CH:29]=2)=[CH:31][C:32]2[C:41](=[CH:40][C:39]4[C:34]([CH:33]=2)=[CH:35][C:36]([CH3:48])=[CH:37][CH:38]=4)[CH:42]=3)[CH:46]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric Acid2회HCID 7966CyclohexanolHCID 61289Aluminum sec-butoxideHCID 22269443HCID 22269443, 화합물

생성물 1

HCID 11460950HCID 11460950, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
145 °C

실험 절차

To a 500 mL three necked round bottom flask with a thermometer, and a distillation head was added 32.76 grams of aluminum tri(sec-butoxide) and 200 mLs of cyclohexanol. To this was added 9 grams 3,10-Dimethylpentacene-5,12-dione. The reaction mixture was heated to 145° C. At 140° C., 8.7 grams of a distillate was collected. The reaction mixture was heated at 140° C. for 43 hours and cooled to room temperature. A solid was isolated by centrifugation. The supernate liquid was poured off and the solid was slurried with 140 mLs of 1N HCl and isolated on a Buchner funnel. The solid was slurried three times with 100 mLs each 1N HCl and the solvent was poured off each time. The solid was slurried three times with 100 mLs of acetone and isolated by filtration. The solid was slurried three times with 100 mLs of THF and isolated by filtration. The residue was air dried to give 2,9-dimethylpentacene.

후처리

  1. distillationAt 140° C., 8.7 grams of a distillate was collected
  2. temperatureThe reaction mixture was heated at 140° C. for 43 hours
  3. temperaturecooled to room temperature
  4. customA solid was isolated by centrifugation
  5. additionThe supernate liquid was poured off
  6. customisolated on a Buchner funnel
  7. additionthe solvent was poured off each time
  8. customisolated by filtration
  9. customisolated by filtration
  10. customdried

출처 및 근거

ORD 기록
ord-f284e0ee4ae84db88b9349c17cf1dbc0
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06974877B2

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