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Toluene → HCID 67366556, 화합물

HRID 2189207
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HRID 2189207 반응식
C1(C)C=CC=CC=1.C([O-])([O-])=O.[Na+].[Na+].Cl[C:15]1[N:24]=[C:23]([NH:25][C@H:26]2[CH2:30][CH2:29][N:28]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:27]2)[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:16]=1.[CH3:38][C:39]1[CH:40]=[CH:41][C:42]([O:48][CH3:49])=[C:43](B(O)O)[CH:44]=1>O.C(O)CCC>[CH3:49][O:48][C:42]1[CH:43]=[CH:44][C:39]([CH3:38])=[CH:40][C:41]=1[C:15]1[N:24]=[C:23]([NH:25][C@H:26]2[CH2:30][CH2:29][N:28]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:27]2)[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 2773485(2-Methoxy-5-methylphenyl)boronic acidHCID 58394359HCID 58394359, 화합물

생성물 1

HCID 67366556HCID 67366556, 화합물수율 99%

시약·촉매·용매 2

HCID 2631-Butanol용매
HCID 962
Water
용매

실험 절차

A mixture of toluene (1.8 mL), n-butanol (3 mL) and 2M Na2CO3 (3 mL) was degassed with a stream of nitrogen for 20 minutes. The mixture was transferred onto a degassed mixture of (S)-tert-butyl 3-(2-chloroquinazolin-4-ylamino)pyrrolidine-1-carboxylate (0.300 g, 0.86 mmol), palladium tetrakistriphenyl phosphine (0.0718 g, 0.06 mmol) and 5-methyl-2-methoxyphenylboronic acid (0.143 g, 0.86 mmol) and the solution was heated at reflux. After 17 hours the reaction was cooled, diluted with water (20 mL), and extracted with ethyl acetate (2×20 mL). The combined organic extracts were washed with brine (20 mL), dried (MgSO4), and concentrated. Silica chromatography (6:1-1:1 petroleum ether/ethyl acetate) gave the title compound as a colourless solid (0.329 g, 99%).

후처리

  1. customwas degassed with a stream of nitrogen for 20 minutes
  2. temperaturethe solution was heated
  3. temperatureat reflux
  4. temperatureAfter 17 hours the reaction was cooled
  5. extractionextracted with ethyl acetate (2×20 mL)
  6. washThe combined organic extracts were washed with brine (20 mL)
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2e2dee760f9249cba88513f4b177835b
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08324226B2

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