Water → HCID 86603585, 화합물

HRID 16645

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HRID 16645 반응식
[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][C:7]=1[C:14](=[O:22])[CH2:15]P(=O)([O-])OCC)[CH:2]([CH3:4])[CH3:3].CC(C)([O-])C.[K+].[CH3:29]/[C:30](/[CH:37]=O)=[CH:31]\[C:32]([O:34][CH2:35][CH3:36])=[O:33].O>O1CCCC1>[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[CH:8][C:7]=1[C:14](=[O:22])[CH:15]=[CH:29][C:30]([CH3:37])=[CH:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:2]([CH3:3])[CH3:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 6009828Ethyl (2E)-3-methyl-4-oxo-2-butenoateHCID 23665647Potassium tert-butoxideHCID 86603586HCID 86603586, 화합물

생성물 1

HCID 86603585HCID 86603585, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
50 °C

실험 절차

3 g (8.4 mmol) of ethyl [2-(2-isobutoxy-5-methoxyphenyl)-2-oxoethyl]-phosphonate dissolved in 20 ml of tetrahydrofuran are added dropwise to a suspension of 1.41 g (12.6 mmol) of potassium tert-butoxide in 30 ml of tetrahydrofuran, heated to 50° C. Heating is continued for 20 minutes at 50° C., the mixture is then cooled to 0° C. and 1.8 g (12.6 mmol) of ethyl 3-methyl-4-oxocrotonate dissolved in 20 ml of tetrahydrofuran are added dropwise. The reaction mixture is then stirred for 72 hours at 25° C. Water is added and the resulting mixture is extracted with ether. After drying (Na2SO4), the solvent is evaporated off and the residue is purified by flash chromatography (dichloromethane) (2.58 g of yellow oil; 89%).

후처리

  1. temperatureHeating
  2. temperaturethe mixture is then cooled to 0° C.
  3. additionare added dropwise
  4. extractionthe resulting mixture is extracted with ether
  5. dry with materialAfter drying (Na2SO4)
  6. customthe solvent is evaporated off
  7. customthe residue is purified by flash chromatography (dichloromethane) (2.58 g of yellow oil; 89%)

출처 및 근거

ORD 기록
ord-a324b16e61e64ab7b1a0c8ce6fe558cf
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737176B2

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