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Diethyl Ether → HCID 131722977, 화합물

HRID 428819
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HRID 428819 반응식
[OH:1][C:2]([CH3:23])([CH2:19][CH2:20][CH2:21][CH3:22])[CH2:3]/[CH:4]=[CH:5]/[Sn](CCCC)(CCCC)CCCC.C(OCC)C.C[Li].[Cu]C#N.[Si:34]([O:41][CH:42]1[CH2:46][C:45](=[O:47])[C:44]([CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][C:54]([O:56][CH3:57])=[O:55])=[CH:43]1)([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:36])[CH3:35].[Cl-].[NH4+]>O1CCCC1>[CH3:57][O:56][C:54](=[O:55])[CH2:53][CH2:52][CH2:51][CH2:50][CH2:49][CH2:48][C@@H:44]1[C@@H:43](/[CH:5]=[CH:4]/[CH2:3][C:2]([OH:1])([CH3:23])[CH2:19][CH2:20][CH2:21][CH3:22])[CH:42]([O:41][Si:34]([C:37]([CH3:40])([CH3:39])[CH3:38])([CH3:35])[CH3:36])[CH2:46][C:45]1=[O:47]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 3283Diethyl EtherHCID 25517Ammonium ChlorideHCID 4653916Methyl 7-(3-((tert-butyldimethylsilyl)oxy)-5-oxocyclopent-1-en-1-yl)heptanoateHCID 11026395HCID 11026395, 화합물HCID 178418348HCID 178418348, 화합물HCID 178418546HCID 178418546, 화합물

생성물 1

HCID 131722977
HCID 131722977, 화합물
수율 75.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Into a dry flask was placed a solution of [(4RS, 1E)-4-hydroxy-4-methyl-1-octenyl]tri-n-butyltin (973 mg, 2.26 mmol) in dry tetrahydrofuran (5 ml) under nitrogen atmosphere and the mixture was cooled to 0° C. The solution was dropped with 5.1 ml (4.48 mmol) of a diethyl ether solution of methyllithium (0.88 mol/liter), warmed to room temperature and stirred for 2 h. After cooling to −40° C., copper (I) cyanide (200 mg, 2.26 mmol) was added and dissolved by letting the temperature rise gradually to 0° C. The reaction liquid was cooled to −78° C., dropped with boron trifluoride ether complex (283 μl, 2.26 mmol), stirred for 10 min and added with a solution of (±) methyl 7-(3-tert-butyldimethylsilyloxy-5-oxo-1-cyclopentenyl)heptanoate (500 mg, 1.4 mmol) in dry tetrahydrofuran (2 ml) was rapidly added. After stirring for 30 min , 20 ml of a saturated aqueous ammonium chloride/aqueous ammonia (9:1) was added, and stirring was continued for 20 min, letting the temperature rise gradually to room temperature. This mixture was extracted with ethyl acetate (70 ml) two times, and the combined organic layer was washed with a saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and concentrated in vacuo to remove solvent. The residue was purified by silica gel column chromatography [ethyl acetate/hexane (1/5)] to give 522 mg (75% yield) of (±)-methyl(16RS, 13E)-11-tert-butyldimethylsilyloxy-16-hydroxy-16-methyl-9-oxoprost-13-en-1-oate as a colorless oil. The spectral data of IR and 1H NMR were identical with those of the example 2.

후처리

  1. customInto a dry flask was placed
  2. temperatureAfter cooling to −40° C.
  3. dissolutiondissolved
  4. customgradually to 0° C
  5. customThe reaction liquid
  6. temperaturewas cooled to −78° C.
  7. additiondropped with boron trifluoride ether complex (283 μl, 2.26 mmol)
  8. stirringstirred for 10 min
  9. additionwas rapidly added
  10. stirringAfter stirring for 30 min
  11. stirringstirring
  12. waitwas continued for 20 min
  13. customgradually to room temperature
  14. extractionThis mixture was extracted with ethyl acetate (70 ml) two times
  15. washthe combined organic layer was washed with a saturated aqueous sodium chloride
  16. dry with materialdried over anhydrous magnesium sulfate
  17. concentrationconcentrated in vacuo
  18. customto remove solvent
  19. customThe residue was purified by silica gel column chromatography [ethyl acetate/hexane (1/5)]

출처 및 근거

ORD 기록
ord-0622e88e35b147b2b02e62b93c24dc03
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06313341B1

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