Hexane → HCID 178506790, 화합물

HRID 68200노트

반응식

HRID 68200 반응식
[C:1]1([C:7]#[CH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Li:9]CCCC.CCCCCC>C1COCC1>[Li:9][C:8]#[C:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 8058HexaneHCID 10821PhenylacetyleneHCID 178418339Butyllithium

생성물 1

HCID 178506790HCID 178506790, 화합물수율 45%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of fresh LiC≡CPh was prepared by reacting 0.057 mL of phenylacetylene (0.525 mmol) and 0.298 mL of 1.5M nBuLi in hexane solution (0.462 mmol) in 15 mL of dry THF at −78° C. for 0.5 hour. The resulting solution was added drop wise via cannula to a solution of 160 mg of Ir(ppy)2(CNtBu)OTf (0.22 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 and the crude was extracted with diethylether. 67.8 mg of Ir(ppy)2(CNtBu)(CCPh) is obtained (45% yield).

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
  5. extractionthe crude was extracted with diethylether

출처 및 근거

ORD 기록
ord-8d12691b227548f1baa85a9b80aede5b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822042B2

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