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Ethylcyclopentadiene → HCID 178438266, 화합물

HRID 735299
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반응식

HRID 735299 반응식
[BH4-].[Na+].[CH2:3]([C:5]1([Li])[CH:9]=[CH:8][CH:7]=[CH:6]1)[CH3:4].[CH2:11]([C:13]1[CH2:17][CH:16]=[CH:15][CH:14]=1)[CH3:12].C([Li])CCC.[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Ta+5:28]>C1COCC1>[CH2:3]([C:5]1([TaH3:28][C:13]2([CH2:11][CH3:12])[CH:17]=[CH:16][CH:15]=[CH:14]2)[CH:9]=[CH:8][CH:7]=[CH:6]1)[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 528166EthylcyclopentadieneHCID 4311764Sodium borohydrideHCID 10269745Tantalum chlorideHCID 178418339ButyllithiumHCID 178506694HCID 178506694, 화합물

생성물 1

HCID 178438266HCID 178438266, 화합물수율 34.2%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

6.85 g (181 mmol) of sodium borohydride and 40 ml of THF were added to a solution of 48.9 g (489 mmol) of ethylcyclopentadienyl lithium prepared from ethylcyclopentadiene and butyl lithium in THF (200 ml), followed by ice-cooling. 24.9 g (69 mmol) of tantalum pentachloride was added to the mixture, followed by refluxing for 4 hours. The solvent was distilled away in vacuo, and the residue was sublimated at 2.5 Pa/100° C. to obtain 8.80 g (yield: 34.2%) of a white solid.

후처리

  1. temperaturecooling
  2. temperatureby refluxing for 4 hours
  3. distillationThe solvent was distilled away in vacuo
  4. customwas sublimated at 2.5 Pa/100° C.

출처 및 근거

ORD 기록
ord-b2f3040dfb7a4e78855225c9e59dd5df
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07592471B2

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