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Sodium Carbonate → HCID 87972489, 화합물

HRID 2180558
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HRID 2180558 반응식
BrC1C=[C:4]2[C:9](=[CH:10]C=1OCC)[C:8]([CH3:16])([CH3:15])[CH2:7][CH:6]=[C:5]2[C:17]([CH3:20])([CH3:19])[CH3:18].B1(B2O[C:33]([CH3:36])([CH3:35])[C:32]([CH3:38])([CH3:37])O2)OC(C)(C)C(C)(C)O1.[C:39]([O-])(=[O:41])[CH3:40].[K+].C(C1C2C=C(B3OC(C)(C)C(C)(C)O3)C(OCC)=CC=2C(C)(C)CC=1)(C)(C)C.I/C(/C)=C\[CH:75]=[CH:76]\[C:77](\[CH3:84])=[CH:78]\[C:79]([O:81][CH2:82][CH3:83])=[O:80].C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O.C1(C)C=CC=CC=1.C(O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:17]([C:5]1[C:4]2[CH:37]=[C:32](/[C:33](/[CH3:35])=[CH:36]\[CH:75]=[CH:76]\[C:77](\[CH3:84])=[CH:78]\[C:79]([O:81][CH2:82][CH3:83])=[O:80])[C:38]([O:41][CH2:39][CH3:40])=[CH:10][C:9]=2[C:8]([CH3:15])([CH3:16])[CH2:7][CH:6]=1)([CH3:18])([CH3:19])[CH3:20]
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참가 물질

11

반응물 6

HCID 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 22490955HCID 22490955, 화합물HCID 69729649HCID 69729649, 화합물HCID 87972285HCID 87972285, 화합물

생성물 1

HCID 87972489
HCID 87972489, 화합물

시약·촉매·용매 4

HCID 178418397HCID 178418397, 화합물촉매HCID 702Ethanol용매HCID 1140Toluene용매HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

A solution of 6-bromo-4-tert-butyl-7-ethoxy-1,1-dimethyl-1,2-dihydronaphthalene (Compound A-6, 350 mg, 1.04 mmol), bis(pinacolato)diboron (370 mg, 1.46 mmol), and potassium acetate (305 mg, 3.12 mmol) in dimethylformamide (8 mL) was purged with argon for 15 minutes. [1, 1-bis(disphenylphosphino)ferrocene]dichloropalladium(II) (1:1 complex with dichloromethane, 82 mg, 0.1 mmol) was added and purged with argon for another 5 min. The reaction was continuously stirred at 80° C. for 4 days under argon. Thereafter the reaction was cooled to room temperature and quenched with water. The reaction mixture was extracted with ethyl acetate. The organic layer was washed successively with water, brine, dried over Na2SO4, and concentrated in vacuo. Purification by column chromatography (silica gel, 10 to 20% ethyl acetate in hexane) yielded a mixture of 2-(8-tert-butyl-3-ethoxy-5,5-dimethyl-5,6-dihydronaphthalen-2-yl)-4,4,5,5-tetramethyl [1,3,2]dioxaborolane (Compound A-8) and 2-(8-tert-butyl-1-(3-ethoxy-5,5-dimethyl-5,6-dihydro-naphthalen-2-yl)boronic acid (Compound A-10). The above mixture of Compounds A-8 and A-10, ethyl 7-iodo-3-methyl-octa-2E,4E,6Z-trienoate (Compound A-11, 130 mg, 0.43 mmol), tetrakis(triphenylphosphine)palladium(0) (40 mg, 0.03 mmol), and 2M sodium carbonate (1 mL, 2 mmol) in toluene (4 mL) and ethanol (2 mL) was heated to 100° C. for 40 h. The reaction was cooled to room temperature and extracted with ethyl acetate. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. Purification by column chromatography (silica gel 1% to 2% ethyl acetate in hexane) yielded the title compound as an oil.

후처리

  1. custompurged with argon for another 5 min
  2. temperatureThereafter the reaction was cooled to room temperature
  3. customquenched with water
  4. extractionThe reaction mixture was extracted with ethyl acetate
  5. washThe organic layer was washed successively with water, brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated in vacuo
  8. customPurification by column chromatography (silica gel, 10 to 20% ethyl acetate in hexane)
  9. customyielded
  10. additionThe above mixture of Compounds
  11. temperatureThe reaction was cooled to room temperature
  12. extractionextracted with ethyl acetate
  13. washThe organic layer was washed with brine
  14. dry with materialdried over Na2SO4
  15. concentrationconcentrated in vacuo
  16. customPurification by column chromatography (silica gel 1% to 2% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-84eed7b1426d4a83ae3f5c449d29a6d9
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06887896B1

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