Phenylacetylene → HCID 178506790, 화합물

HRID 68201

반응식

HRID 68201 반응식
[C:1]1([C:7]#[CH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CCCCCC.[Li:15]CCCC>C1COCC1>[Li:15][C:8]#[C:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 10821PhenylacetyleneHCID 178418244HCID 178418244, 화합물

생성물 1

HCID 178506790HCID 178506790, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of fresh LiC≡CPh was prepared by reacting 0.118 mL of phenylacetylene (1.08 mmol) and 0.48 mL of 1.5M hexane nBuLi solution (0.72 mmol) in 50 mL of dry THF at −78° C. for 0.5 hour. The solution was added drop wise via cannula to a solution of 150 mg of Ir(ppy)2(MeOH)2OTf (0.18 mmol) in 10 mL of dry THF at −78° C. The mixture was reacted for 1 h at −78° C. and the temperature was raised to RT over 2 hours. The solvent was removed under reduced pressure obtaining the Ir(ppy)2(CCPh)2Li.

후처리

  1. customat −78° C.
  2. customfor 0.5 hour
  3. customThe mixture was reacted for 1 h at −78° C.
  4. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-bce394fd86704cb8aed12f57cc631d5d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822042B2

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