Hydrochloric Acid → HCID 9837536, 화합물

HRID 1582760노트

반응식

HRID 1582760 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

HCID 9837536HCID 9837536, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6386tert-Butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3713e5a1983840919374fc8fd6b89894
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06737425B1

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