Hexane → HCID 131725129, 화합물

HRID 271006

반응식

HRID 271006 반응식
[C:1]([C:5]1[CH:6]=[CH:7][C:8]2[CH2:9][C:10]3[C:15]([C:16]=2[CH:17]=1)=[CH:14][C:13]([C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:12][CH:11]=3)([CH3:4])([CH3:3])[CH3:2].CCCCCC.C([Li])CCC.[CH3:33][C:34]([CH3:40])=[C:35]1[CH:39]=[CH:38][CH:37]=[CH:36]1>C1COCC1.O>[CH:35]1([C:34]([C:11]2[C:10]3[CH2:9][C:8]4[C:16](=[CH:17][C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:6][CH:7]=4)[C:15]=3[CH:14]=[C:13]([C:18]([CH3:21])([CH3:20])[CH3:19])[CH:12]=2)([CH3:40])[CH3:33])[CH:39]=[CH:38][CH:37]=[CH:36]1

참가 물질

7

반응물 4

HCID 8058HexaneHCID 1374671,3-Cyclopentadiene, 5-(1-methylethylidene)-HCID 111404373,6-DI-Tert-butylfluoreneHCID 178418339Butyllithium

생성물 1

HCID 131725129HCID 131725129, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매3회

실험 절차

To a solution of 3.0 g (10.8 mmol) of 3,6-di-tert-butylfluorene in 40 ml of THF, 7.0 ml (11.3 mmol) of a hexane solution of n-butyllithium was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for 6 hours. From the reaction mixture, the solvent was removed under reduced pressure, and the residue was washed with pentane and dried to obtain a white solid. To a solution of the solid in 30 ml of THF, a solution of 1.4 g (13.2 mmol) of 6,6-dimethylfulvene in 30 ml of THF was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring for 5 hours. Then, 30 ml of water-was added. The organic phase extracted with diethyl ether and separated was dried over magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a solid. The solid was recrystallized from methanol to obtain 2.9 g of a slightly yellow solid. The analyzed values are given below.

후처리

  1. customFrom the reaction mixture, the solvent was removed under reduced pressure
  2. washthe residue was washed with pentane
  3. customdried
  4. customto obtain a white solid
  5. stirringby stirring for 5 hours
  6. extractionThe organic phase extracted with diethyl ether
  7. customseparated
  8. dry with materialwas dried over magnesium sulfate
  9. filtrationfiltered
  10. customFrom the filtrate, the solvent was removed under reduced pressure
  11. customto obtain a solid
  12. customThe solid was recrystallized from methanol
  13. customto obtain 2.9 g of a slightly yellow solid

출처 및 근거

ORD 기록
ord-814432f761564d03a0bf5da5d1582fde
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449533B2

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