Toluene → HCID 58769446, 화합물

HRID 418031

반응식

HRID 418031 반응식
[CH:1]1[C:18]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.I[C:20]1[CH:25]=[CH:24][CH:23]=[C:22](I)[CH:21]=1.C(=O)([O-])[O-].[K+].[K+].[C:33]1([CH3:39])[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1>O>[CH:4]1[C:5]2[C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[C:12]3[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:18]=2[CH:1]=[CH:2][C:3]=1[C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([C:35]2[CH:36]=[CH:37][C:38]3[C:18]4[C:5](=[CH:4][CH:3]=[CH:2][CH:1]=4)[C:6]4[C:39](=[CH:10][CH:9]=[CH:8][CH:7]=4)[C:33]=3[CH:34]=2)[CH:21]=1

참가 물질

6

반응물 4

HCID 1140TolueneHCID 9170TriphenyleneHCID 11430Potassium CarbonateHCID 12270Benzene, 1,3-diiodo-

생성물 1

HCID 58769446HCID 58769446, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
87 °C

실험 절차

1.23 g (3.5 mmol) of the triphenylene moronic ester from the previous step, 0.5 g (1.5 mmol) of 1,3-diiodobenzene, 1.0 g (7.5 mmol) of potassium carbonate, 30 mL of toluene, and 10 mL of water was mixed in a 250 mL three-neck flask. The system was purged by nitrogen for 10 min before adding 0.05 g of Pd(PPh3)4. The mixture was then heated up to 87° C. with vigorous stirring. After 24 hr, to the mixture was added 200 mL of methanol. The precipitate was collected by filtration. The solid was washed with copious amount of methanol, then hexanes. The solid was then recrystallized from 80 ml of xylenes. Final purification of the product involved subliming the material at 250° C. 0.35 g product was collected as white needle crystals.

후처리

  1. customThe system was purged by nitrogen for 10 min
  2. additionbefore adding 0.05 g of Pd(PPh3)4
  3. additionto the mixture was added 200 mL of methanol
  4. filtrationThe precipitate was collected by filtration
  5. washThe solid was washed with copious amount of methanol
  6. customThe solid was then recrystallized from 80 ml of xylenes
  7. customFinal purification of the product
  8. customat 250° C
  9. custom0.35 g product was collected as white needle crystals

출처 및 근거

ORD 기록
ord-08cdd25534ec478b9be339a85721ed6d
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08092924B2

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