3-Methyl-2-butanone → HCID 59487984, 화합물

HRID 1881392노트

반응식

HRID 1881392 반응식
C(OC(=O)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=[O:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)C.C[C:21](C)([O-:23])C.[K+].[CH3:26][CH:27]([CH3:31])[C:28](=[O:30])[CH3:29]>C1COCC1>[C:11]([C:6]1[CH:5]=[CH:10][C:9]([C:21](=[O:23])[CH2:29][C:28](=[O:30])[CH:27]([CH3:31])[CH3:26])=[CH:8][CH:7]=1)(=[O:18])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

참가 물질

5

반응물 3

HCID 112513-Methyl-2-butanoneHCID 221768Ethyl o-benzoylbenzoateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 59487984HCID 59487984, 화합물수율 87.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

10 g (39 mmol) of benzoylbenzoic ethylester are added to a suspension of 3.94 g (35 mmol) of potassium-tert-butoxid in 60 ml of THF at 0° C. under argon. 2.82 g (33 mmol) of 3-methyl-2-butanone are added in 1 h while the temperature rises to 25° C. After 2 h at 40° C. the reaction mixture is poured into 500 ml of ice water containing 10 ml conc. HCl. Extraction with toluene and evaporation gives the crude product (8.5 g) which is purified by crystallisation in heptane yielding 3.7 g of a white solid. The structure is confirmed by 1H-NMR and 13C-NMR spectra. mp: 76.5-78° C.

후처리

  1. customrises to 25° C
  2. extractionExtraction
  3. customwith toluene and evaporation

출처 및 근거

ORD 기록
ord-68b8389eaf4b4f6dbfe03b8110b546cd
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318830B2

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