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4-Pentynoic acid, 3,3-dimethyl-, ethyl ester → Ethyl 5-(2-amino-4-fluoro-5-nitrophenyl)-3,3-dimethylpent-4-ynoate

HRID 1847585
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HRID 1847585 반응식
Br[C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[C:6]([F:12])=[CH:5][C:3]=1[NH2:4].[CH3:13][C:14]([CH3:23])([C:21]#[CH:22])[CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17]>CCN(CC)CC.C(OCC)(=O)C.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu]I>[CH2:19]([O:18][C:16](=[O:17])[CH2:15][C:14]([CH3:23])([CH3:13])[C:21]#[C:22][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[C:6]([F:12])=[CH:5][C:3]=1[NH2:4])[CH3:20]
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참가 물질

8

반응물 2

HCID 100577294-Pentynoic acid, 3,3-dimethyl-, ethyl esterHCID 574885132-Bromo-5-fluoro-4-nitroaniline

생성물 1

HCID 59129516Ethyl 5-(2-amino-4-fluoro-5-nitrophenyl)-3,3-dimethylpent-4-ynoate수율 58.9%

시약·촉매·용매 5

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매
HCID 178418476
HCID 178418476, 화합물
촉매
HCID 962Water용매
HCID 8471Triethylamine용매
HCID 8857Ethyl Acetate용매

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온도
70 °C

실험 절차

To a solution of 2-bromo-5-fluoro-4-nitroaniline (45.7 g, 0.19 mol) and ethyl 3,3-dimethylpent-4-ynoate (88.3 g, 0.57 mol) in Et3N (700 mL) was added Pd(PPh3)2Cl2 (13.8 g, 0.02 mol) and CuI (3.6 g, 0.02 mol) under N2. The reaction mixture was stirred at 70° C. for 8 hours. The reaction mixture was diluted with 500 mL of ethyl acetate and 1500 mL of water. The organic layer was separated and the aqueous phase was extracted with ethyl acetate (500 mL×3), the combined organic layers were washed with brine and dried over anhydrous Na2SO4, filtered and evaporated under reduced pressure and the residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate 10:1) to give ethyl-5-(2-amino-4-fluoro-5-nitrophenyl)-3,3-dimethylpent-4-ynoate (34.5 g, 57%). 1H NMR (300 MHz, CDCl3) δ 8.05 (d, J=8.1 Hz, 1H), 6.36 (d, J=13.2 Hz, 1H), 5.60 (brs, 2H), 4.16 (q, J=7.2 Hz, 2H), 2.51 (s, 2H), 1.40 (s, 6H), 1.28 (t, J=7.2 Hz, 3H).

후처리

  1. customThe organic layer was separated
  2. extractionthe aqueous phase was extracted with ethyl acetate (500 mL×3)
  3. washthe combined organic layers were washed with brine
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customthe residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate 10:1)

출처 및 근거

ORD 기록
ord-12a833ec724541dda3c8a8619ad8c2ae
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952050B2

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