3-Methyl-2-butanone → HCID 59487984、化合物

HRID 1881392ノート

反応式

HRID 1881392 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 59487984HCID 59487984、化合物収率 87.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-68b8389eaf4b4f6dbfe03b8110b546cd
出典データセット
uspto-grants-2012_11
特許番号
US08318830B2

反応ノート

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