Hydrochloric Acid → 9-Ethynyl-9-fluorenol

HRID 1734125노트

반응식

HRID 1734125 반응식
[CH:1]1[C:13]2[C:12](=[O:14])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH2:15]1COC[CH2:16]1.[C-]#[C-].[Na+].[Na+].Cl>C1(C)C(C)=CC=CC=1>[C:15]([C:12]1([OH:14])[C:13]2[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=2[C:6]2[C:11]1=[CH:10][CH:9]=[CH:8][CH:7]=2)#[CH:16]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 10241FluorenoneHCID 178463197HCID 178463197, 화합물

생성물 1

HCID 5187719-Ethynyl-9-fluorenol

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

9 g (0.05 mol) of 9-fluorenone and 100 ml of anhydrous THF are charged into a dry flask of 250 ml. To the resulting solution a suspension of sodium acetylide [17.8 g (0.0525 mol) in mineral oil/xylene, 18% by weight based on the suspension; solid purity 95%] is added under nitrogen, by means of a syringe. The resulting suspension is kept overnight under nitrogen and with stirring before being poured into 75 ml of 10% HCl. The phases are separated and the aqueous phase is extracted twice with 100 ml of ethyl ether. The organic extracts are combined and thoroughly dried over sodium sulfate. By eliminating the solvent, 10.1 g of product is obtained, which is used without any further purification.

후처리

  1. additionsolid purity 95%] is added under nitrogen, by means of a syringe
  2. customThe phases are separated
  3. extractionthe aqueous phase is extracted twice with 100 ml of ethyl ether
  4. dry with materialthoroughly dried over sodium sulfate

출처 및 근거

ORD 기록
ord-482d3d186f19497fa94ffade5005a094
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532361

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