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Sodium Carbonate → 1-[4-(2-Butoxy-3,5-diisopropyl-phenyl)quinolin-6-yl]-ethanone

HRID 1394627
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HRID 1394627 반응식
[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[CH:9][CH:8]=[C:7]2OS(C(F)(F)F)(=O)=O)(=[O:3])[CH3:2].[CH2:22]([O:26][C:27]1[C:32]([CH:33]([CH3:35])[CH3:34])=[CH:31][C:30]([CH:36]([CH3:38])[CH3:37])=[CH:29][C:28]=1B(O)O)[CH2:23][CH2:24][CH3:25].C([O-])([O-])=O.[Na+].[Na+]>C1(C)C=CC=CC=1.[Cl-].[Na+].O.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>[CH2:22]([O:26][C:27]1[C:32]([CH:33]([CH3:35])[CH3:34])=[CH:31][C:30]([CH:36]([CH3:37])[CH3:38])=[CH:29][C:28]=1[C:7]1[C:6]2[C:11](=[CH:12][CH:13]=[C:4]([C:1](=[O:3])[CH3:2])[CH:5]=2)[N:10]=[CH:9][CH:8]=1)[CH2:23][CH2:24][CH3:25]
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참가 물질

7

반응물 3

HCID 10340Sodium CarbonateHCID 17952696(2-Butoxy-3,5-diisopropylphenyl)-boronic acidHCID 59682072Trifluoro-methanesulfonic acid 6-acetyl-quinolin-4-yl ester

생성물 1

HCID 596820521-[4-(2-Butoxy-3,5-diisopropyl-phenyl)quinolin-6-yl]-ethanone수율 93%

시약·촉매·용매 3

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 1140Toluene용매
HCID 57417360Sodium chloride; water용매

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온도
80 °C

실험 절차

To a solution of trifluoro-methanesulfonic acid 6-acetyl-quinolin-4-yl ester (321.7 mg, 1.008 mmol) and (2-butoxy-3,5-diisopropyl-phenyl)-boronic acid (315.3 mg, 1.133 mmol) (see Example 17, step B) in toluene (10 mL) was added 2N Na2CO3 (1.1 mL) and Pd(PPh3)4 (117.1 mg, 0.101 mmol). The solution was stirred at 80° C. for 2 h under N2 atm. The mixture was poured into brine (30 mL) and extracted with ethyl acetate (30 mL). The organic phase was dried, filtered, and concentrated. The crude material was purified by flash chromatography (2:8) ethyl acetate:hexanes to give 1-[4-(2-butoxy-3,5-diisopropyl-phenyl)quinolin-6-yl]-ethanone (378 mg, 93% yield) as a light yellow crystalline solid. Mp 132.8° C. 1H NMR (400 MHz, DMSO-d6): δ 9.01 (d, 1H, J=4.4), 8.40 (d, 1H, J=2.0), 8.25 (2d, 1H, J=2.0, 8.8), 8.16 (d, 1H, J=8.8), 7.50 (d, 1H, J=4.4), 7.24 (m, 1H), 7.00 (d, 1H, J=2.4),3.36 (m, 1H), 3.26 (m, 1H), 3.16 (m, 1H), 2.94 (m, 1H), 2.58 (s, 3H), 1.29 (m, 12H), 1.10 (m, 2H), 0.79 (m, 2H), 0.47 (t, 3H, J=7.3). 13C NMR (75 MHz, DMSO-d6): δ 197.1, 152.3, 151.6, 149.6, 147.2, 144.2, 141.6, 134.0, 129.7, 128.5, 127.2, 126.5, 125.4, 123.0, 73.0, 33.0, 31.1, 26.4, 24.0, 23.9, 23.8, 23.0, 17.9, 12.9. IR (CHCl3, cm−1): 2963, 2934, 2872, 1681. MS [EI+] 404 (M+H)+. Analytical (C27H33NO2): Calculated C, 80.36; H, 8.24; N, 3.47. Found: C, 79.98; H, 8.57; N, 3.46.

후처리

  1. extractionextracted with ethyl acetate (30 mL)
  2. customThe organic phase was dried
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude material was purified by flash chromatography (2:8) ethyl acetate

출처 및 근거

ORD 기록
ord-f15559d00db0480097480f8cc3d688f8
출처 데이터셋
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07348359B2

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