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Diisopropylamine → Ethyl 2-dimethylamino-5-ethoxycarbonyl-2,4-tridecadienoate

HRID 477318
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HRID 477318 반응식
[C:1]([O:12][CH2:13][CH3:14])(=[O:11])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].C(NC(C)C)(C)C.C([Li])CCC.F[B-](F)(F)F.[CH3:32][N:33]([CH3:45])[C:34]([C:40]([O:42][CH2:43][CH3:44])=[O:41])=[CH:35][CH:36]=[N+](C)C.[Cl-].[NH4+]>CCCCCC.O1CCCC1.O.ClCCl>[CH3:32][N:33]([CH3:45])[C:34](=[CH:35][CH:36]=[C:2]([C:1]([O:12][CH2:13][CH3:14])=[O:11])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])[C:40]([O:42][CH2:43][CH3:44])=[O:41]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 7912DiisopropylamineHCID 8048Ethyl caprateHCID 25517Ammonium ChlorideHCID 86743575N-(dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborateHCID 178418339Butyllithium

생성물 1

HCID 54180968Ethyl 2-dimethylamino-5-ethoxycarbonyl-2,4-tridecadienoate
수율 55.5%

시약·촉매·용매 4

HCID 962Water용매2회HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매

반응 조건

온도
-78 °C

실험 절차

Ethyl n-decanoate (10 g) is added in the course of 10 minutes at a temperature in the region of -78° C. to a stirred mixture of diisopropylamine (5.6 cc), a 1.6M solution (37.5 cc) of n-butyllithium in hexane and tetrahydrofuran (30 cc). Stirring is maintained for 30 minutes at the same temperature, N-(3-dimethylamino-3-ethoxycarbonylpropenylidene)-N-methylmethanaminium tetrafluoroborate (14.3 g) is then added and stirring is maintained for 3 hours at a temperature in the region of -78° C. After a gradual warming to approximately 20° C., ammonium chloride (4 g) dissolved in water (50 cc) is added to the reaction medium. Dichloromethane (200 cc) and water (100 cc) are added, and the organic phase is separated off after settling has taken place. The aqueous phase is washed with dichloromethane (2×50 cc). The organic phases are combined, dried over anhydrous magnesium sulphate, filtered and evaporated at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa). The residue is dissolved in a mixture (30 cc) of cyclohexane and ethyl acetate (60:40 by volume), and the solution obtained is poured onto silica (600 g) contained in a column 7 cm in diameter. Elution is performed with a mixture of cyclohexane and ethyl acetate (60:40 by volume), and the eluate is concentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa). Ethyl 2-dimethylamino-5-ethoxycarbonyl-2,4-tridecadienoate (9.8 g) is thereby obtained, and is used in the crude state in the subsequent syntheses.

후처리

  1. additionis then added
  2. stirringstirring
  3. temperatureAfter a gradual warming to approximately 20° C.
  4. additionis added to the reaction medium
  5. customthe organic phase is separated off after settling
  6. washThe aqueous phase is washed with dichloromethane (2×50 cc)
  7. dry with materialdried over anhydrous magnesium sulphate
  8. filtrationfiltered
  9. customevaporated at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa)
  10. dissolutionThe residue is dissolved in a mixture (30 cc) of cyclohexane and ethyl acetate (60:40 by volume)
  11. customthe solution obtained
  12. additionis poured onto silica (600 g)
  13. washElution
  14. additionis performed with a mixture of cyclohexane and ethyl acetate (60:40 by volume)
  15. concentrationthe eluate is concentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa)

출처 및 근거

ORD 기록
ord-5572d205a54a4e02bfbdd967f1f4a3f5
출처 데이터셋
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04886835

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