Hydrochloric Acid → HCID 9837536、化合物

HRID 1582760ノート

反応式

HRID 1582760 の反応式
[CH3:1][CH:2]([C:4]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)([CH2:7][CH2:8][CH:9]=[O:10])[C:5]#[N:6])[CH3:3].P([O-])(O)(O)=[O:18].[Na+].CC(=CC)C.Cl([O-])=O.[Na+].Cl>O.C(O)(C)(C)C>[C:5]([C:4]([C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)([CH:2]([CH3:1])[CH3:3])[CH2:7][CH2:8][C:9]([OH:18])=[O:10])#[N:6]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 105532-Methyl-2-buteneHCID 140258132-(1-Methylethyl)-5-oxo-2-phenylpentane nitrileHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphate

生成物 1

HCID 9837536HCID 9837536、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6386tert-Butanol溶媒

実験手順

2-(1-Methylethyl)-5-oxo-2-phenylpentane nitrile, 6.00 g 27.9 mmol, was dissolved in a mixed solvent of water 55 ml/t-butyl alcohol 200 ml, and sodium dihydrogen phosphate 4.35 g 27.9 mmol and 2-methyl-2-butene 14.8 ml 139 mmol were further added thereto. Sodium chlorite 10.0 g 111 mmol in limited amounts was added thereto and stirred for 2 hours. The reaction mixture was ice-cooled and acidified by 2N hydrochloric acid. Then, it was extracted with ether, washed with dilute hydrochloric acid, dried over magnesium sulfate, and evaporated. The residue was purified by silica gel column chromatography (ethyl acetate/hexane system), whereby the title compound, 4.10 g 17.7 mmol, 63.4%, was obtained as a white solid.

後処理

  1. additionwere further added
  2. temperaturecooled
  3. extractionThen, it was extracted with ether
  4. washwashed with dilute hydrochloric acid
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane system), whereby the title compound, 4.10 g 17.7 mmol, 63.4%
  8. customwas obtained as a white solid

出典と根拠

ORDレコード
ord-3713e5a1983840919374fc8fd6b89894
出典データセット
uspto-grants-2004_05
特許番号
US06737425B1

反応ノート

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