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Cesium carbonate → HCID 89813717, 화합물

HRID 525356
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HRID 525356 반응식
[CH2:1]([C:3]1([CH2:15][CH3:16])[O:7][C:6](=[O:8])[NH:5][C@H:4]1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH3:2].I[C:18]1[CH:36]=[CH:35][C:21]([C:22]([NH:24][C:25]2[CH:26]=[CH:27][CH:28]=[C:29]3[C:34]=2[N:33]=[CH:32][CH:31]=[CH:30]3)=[O:23])=[CH:20][CH:19]=1.C([O-])([O-])=O.[Cs+].[Cs+].CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].O.O1CCOCC1>[CH2:15]([C:3]1([CH2:1][CH3:2])[O:7][C:6](=[O:8])[N:5]([C:18]2[CH:36]=[CH:35][C:21]([C:22]([NH:24][C:25]3[CH:26]=[CH:27][CH:28]=[C:29]4[C:34]=3[N:33]=[CH:32][CH:31]=[CH:30]4)=[O:23])=[CH:20][CH:19]=2)[C@H:4]1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH3:16]
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참가 물질

8

반응물 4

HCID 10796Cesium carbonateHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 41661718HCID 41661718, 화합물HCID 89814220HCID 89814220, 화합물

생성물 1

HCID 89813717HCID 89813717, 화합물수율 7.9%

시약·촉매·용매 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 962Water용매
HCID 312751,4-Dioxane용매

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온도
90 °C

실험 절차

To a 25 mL round bottom flask were added (S)-5,5-diethyl-4-phenyloxazolidin-2-one (0.3 g, 1.36 mmol), 4-iodo-N-(quinolin-8-yl)benzamide (0.560 g, 1.5 mmol), Cs2CO3 (0.972 g, 3.0 mmol), X-Phos (35 mg, 0.068 mmol), Pd2(dba)3 (62 mg, 0.068 mmol) and 1,4-dioxane (2 mL). The mixture was purged with N2 gas for 15 minutes. The reaction mixture was then heated at 90° C. for 6 hours. After completion of reaction (monitored by TLC, TLC eluent: 30% EtOAc in hexane), the reaction mixture was cooled to ambient temperature and treated with water (5 mL) and the mixture extracted with EtOAc (5 mL). The aqueous layer was back extracted with EtOAc (5 mL). The combined organic layers were dried over anhydrous Na2SO4 and concentrated. The crude material was purified with HPLC (column: AG/AD/C18-027, ramping ACN in H2O, 40-50% B, 0-2 minutes, 50-90% B, 2-10 minutes, flow rate 20 mL/min) to afford 50 mg of (S)-4-(5,5-diethyl-2-oxo-4-phenyloxazolidin-3-yl)-N-(quinolin-8-yl)benzamide as a brown solid. 1H NMR (300 MHz, CDCl3) δ: 10.67 (s, 1H), 8.96-8.80 (m, 2H), 8.20 (dd, J=8.3, 1.6 Hz, 1H), 7.99 (d, J=9 Hz, 2H), 7.68 (d, J=8.7 Hz, 2H), 7.62-7.56 (m, 2H), 7.57-7.47 (m, 1H), 7.40-7.36 (m, 3H), 7.28-7.24 (m, 2H), 5.15 (s, 1H), 2.04-1.96 (m, 2H), 1.39-1.20 (m, 2H), 1.12 (t, J=7.5 Hz, 3H), 0.85 (t, J=7.4 Hz, 3H). m/z (ESI) 466.2 (M+H)+.

후처리

  1. customThe mixture was purged with N2 gas for 15 minutes
  2. customAfter completion of reaction (monitored by TLC, TLC eluent: 30% EtOAc in hexane)
  3. temperaturethe reaction mixture was cooled to ambient temperature
  4. extractionthe mixture extracted with EtOAc (5 mL)
  5. extractionThe aqueous layer was back extracted with EtOAc (5 mL)
  6. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  7. concentrationconcentrated
  8. customThe crude material was purified with HPLC (column: AG/AD/C18-027, ramping ACN in H2O, 40-50% B, 0-2 minutes, 50-90% B, 2-10 minutes, flow rate 20 mL/min)

출처 및 근거

ORD 기록
ord-9ba411976d534547b2d850f119b9cb9d
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09340549B2

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