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3,6-DI-Tert-butyl-2,7-bis(chloromethyl)-9H-fluorene → 2,7-Dimethyl-3,6-ditert-butyl-fluorene

HRID 1821154
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HRID 1821154 반응식
Cl[CH2:2][C:3]1[C:15]([C:16]([CH3:19])([CH3:18])[CH3:17])=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9]([CH2:24]Cl)=[C:10]([C:20]([CH3:23])([CH3:22])[CH3:21])[CH:11]=3)[CH2:6][C:5]=2[CH:4]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH3:24][C:9]1[C:10]([C:20]([CH3:21])([CH3:22])[CH3:23])=[CH:11][C:12]2[C:13]3[C:5](=[CH:4][C:3]([CH3:2])=[C:15]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:14]=3)[CH2:6][C:7]=2[CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 149482733,6-DI-Tert-butyl-2,7-bis(chloromethyl)-9H-fluoreneHCID 21226445Aluminium lithium hydride

생성물 1

HCID 219826932,7-Dimethyl-3,6-ditert-butyl-fluorene수율 85%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2,7-dichloromethyl-3,6-di-t-butylfluorene (0.75 g, 2.0 mmol) in THF (15 ml) was added a small portion of LiAlH4 (220 mg, 5.8 mmol) under stirring and the mixture was refluxed for 4 hours. The reaction was quenched with water and NaOH and extracted with ether. The ether solution was evaporated under vacuum to give a white solid of 2,7-di-methyl-3,6-di-tert-butyl-fluorene with a yield of 85%.

후처리

  1. temperaturethe mixture was refluxed for 4 hours
  2. customThe reaction was quenched with water and NaOH
  3. extractionextracted with ether
  4. customThe ether solution was evaporated under vacuum

출처 및 근거

ORD 기록
ord-a84408ae34894c9787965e98019ed3a7
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07605294B2

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