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5-Bromoindole → N-(2-bromo-4-(1-methylethyl)phenyl)-N-ethyl-4-(5-indolylcarbonyl)-6-methylpyrimidinamine

HRID 1251502
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HRID 1251502 반응식
[H-].[K+].Br[C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][CH:8]=[CH:7]2.C([Li])(C)(C)C.[Br:18][C:19]1[CH:24]=[C:23]([CH:25]([CH3:27])[CH3:26])[CH:22]=[CH:21][C:20]=1[N:28]([C:31]1[N:36]=[C:35]([C:37](OC)=[O:38])[CH:34]=[C:33]([CH3:41])[N:32]=1)[CH2:29][CH3:30]>CCOCC.C(OCC)(=O)C>[Br:18][C:19]1[CH:24]=[C:23]([CH:25]([CH3:26])[CH3:27])[CH:22]=[CH:21][C:20]=1[N:28]([CH2:29][CH3:30])[C:31]1[N:36]=[C:35]([C:37]([C:4]2[CH:5]=[C:6]3[C:10](=[CH:11][CH:12]=2)[NH:9][CH:8]=[CH:7]3)=[O:38])[CH:34]=[C:33]([CH3:41])[N:32]=1
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참가 물질

7

반응물 4

HCID 249055-BromoindoleHCID 82127Potassium hydrideHCID 183237072-(N-(2-bromo-4-(2-propyl)phenyl)-N-ethylamino)-4-carbomethoxy-6-methyl-pyrimidineHCID 178418306HCID 178418306, 화합물

생성물 1

HCID 18323781N-(2-bromo-4-(1-methylethyl)phenyl)-N-ethyl-4-(5-indolylcarbonyl)-6-methylpyrimidinamine수율 24%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매3회
HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

To a suspension of potassium hydride (35% in oil, 0.16 g, 1.4 mmol), washed with hexanes and decanted twice, in anhydrous ether (5 mL), cooled to 0° C. under a nitrogen atmosphere was added a solution of 5-bromoindole (0.27 g, 1.4 mmol) in anhydrous ether. After being stirred for 30 min., the reaction mixture was cooled to −78° C. and transferred via cannula to a pre-cooled (−78° C.) mixture of t-butyl lithium (1.7 M in pentane, 1.6 mL, 2.7 mmol) in dry ether (5 mL). The resulting white suspension was stirred at −78° C. for 30 min and a solution of methyl 2-(N-(2-bromo-4-(1-methylethyl)-phenyl)-N-ethylamino)-6-methyl-4-pyrimidinecarboxylate (Example 18) (0.5 g, 1.25 mmol) in anhydrous ether (5 mL) was added dropwise. After quenching the reaction mixture as in Example 87; it was extracted three times with ethyl acetate, followed by two washings of the combined organic layers with a saturated NaHCO3 solution, drying over MgSO4, filtration and concentration in vacuo to give a dark brown oil. Column chromatography (ethyl acetate: hexanes::1:4) afforded the title product, a light brown solid (140 mg, 24% yield, Rf 0.2): mp 77-79° C.; NMR (DMSO-d6, 400 MHz, 90° C.): 11.6-11.35 (br s, 1H), 8.30 (s, 1H), 7.75 (dd, 1H, J=8, 1), 7.55 (d, 1H, J=1), 7.4-7.35 (m, 2H), 7.35-7.25 (m, 2H), 6.9 (s, 1H), 6.60-6.55 (m, 1H), 4.1-3.7 (m, 2H), 2.95-2.8 (m, 1H), 2.4 (br s, 3H), 1.25-1.1 (m, 9H); Anal (C25H25BrN4O): C, 62.90; H, 5.28; N, 11.74; Br, 16.74; Found: C, 63.13; H, 5.60; N, 11.37; Br, 16.80.

후처리

  1. washwashed with hexanes
  2. customdecanted twice, in anhydrous ether (5 mL)
  3. temperaturethe reaction mixture was cooled to −78° C.
  4. temperaturea pre-cooled
  5. stirringThe resulting white suspension was stirred at −78° C. for 30 min
  6. customAfter quenching the reaction mixture as in Example 87
  7. extractionit was extracted three times with ethyl acetate
  8. dry with materialdrying over MgSO4, filtration and concentration in vacuo
  9. customto give a dark brown oil

출처 및 근거

ORD 기록
ord-bbbce212ee084037951001db741cf53b
출처 데이터셋
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06342503B1

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