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3,9-Dimethylpentacene-5,7(12H,14H)-dione → HCID 22269468, 화합물

HRID 488953
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HRID 488953 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:6][C:7]3[C:20]([C:21](=O)[C:22]=2[CH:23]=1)=[CH:19][C:18]1[C:17](=O)[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([CH3:26])[CH:15]=2)[CH2:10][C:9]=1[CH:8]=3>COCCOCCOC>[CH3:26][C:14]1[CH:13]=[CH:12][C:11]2[C:16](=[CH:17][C:18]3[C:9]([CH:10]=2)=[CH:8][C:7]2[C:20](=[CH:21][C:22]4[C:5]([CH:6]=2)=[CH:4][CH:3]=[C:2]([CH3:1])[CH:23]=4)[CH:19]=3)[CH:15]=1
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참가 물질

3

반응물 1

HCID 222694733,9-Dimethylpentacene-5,7(12H,14H)-dione

생성물 1

HCID 22269468HCID 22269468, 화합물

시약·촉매·용매 1

HCID 8150Diglyme용매

반응 조건

온도
60 °C

실험 절차

A mixture of 1 gram of 3,9-dimethylpentacene-5,7(12H,14H)-dione and 10 mL of 2-methoxyethyl ether was stirred and flushed with nitrogen for 15 minutes. To this was added 0.948 grams of sodium borohydride and stirring was continued at room temperature overnight. To the mixture was added 6.3 mL of methanol and stirring was continued for 1.5 hours at room temperature. To the mixture was added 15 mL of acetic acid and 10 mL of concentrated hydrochloric acid. The mixture was stirred for one hour at room temperature followed by heating for one hour at 60° C. To the mixture was added 50 mL of water and the resulting solid was isolated by filtration and washed with water. The solid was washed with tetrahydrofuran until a pale filtrate resulted. The solid was washed with heptane and dried under an atmosphere of nitrogen to give 2,10-dimethylpentacene.

후처리

  1. customflushed with nitrogen for 15 minutes
  2. additionTo this was added 0.948 grams of sodium borohydride
  3. stirringstirring
  4. additionTo the mixture was added 6.3 mL of methanol
  5. stirringstirring
  6. waitwas continued for 1.5 hours at room temperature
  7. additionTo the mixture was added 15 mL of acetic acid and 10 mL of concentrated hydrochloric acid
  8. stirringThe mixture was stirred for one hour at room temperature
  9. additionTo the mixture was added 50 mL of water
  10. customthe resulting solid was isolated by filtration
  11. washwashed with water
  12. washThe solid was washed with tetrahydrofuran until a pale filtrate
  13. customresulted
  14. washThe solid was washed with heptane
  15. customdried under an atmosphere of nitrogen

출처 및 근거

ORD 기록
ord-1e3bb8db210b4808a49c90b5c652e225
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06974877B2

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