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Sodium Carbonate → HCID 87972489、化合物

HRID 2180558
ノート
印刷プレビュー

反応式

HRID 2180558 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

11

反応物 6

HCID 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 22490955HCID 22490955、化合物HCID 69729649HCID 69729649、化合物HCID 87972285HCID 87972285、化合物

生成物 1

HCID 87972489
HCID 87972489、化合物

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒HCID 702Ethanol溶媒HCID 1140Toluene溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-84eed7b1426d4a83ae3f5c449d29a6d9
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06887896B1

反応ノート

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