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Potassium Carbonate → HCID 46842007, 화합물

HRID 1846351
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HRID 1846351 반응식
[C:1]([O-])([O-])=O.[K+].[K+].CB1OB(C)OB(C)O1.Cl[C:17]1[N:22]=[CH:21][C:20]([C:23]2[N:32]([C:33]3[CH:38]=[CH:37][C:36]([CH:39]4[CH2:43][CH2:42][CH2:41][CH2:40]4)=[CH:35][CH:34]=3)[C:31](=[O:44])[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[N:24]=2)=[CH:19][CH:18]=1>O1CCOCC1.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>[CH:39]1([C:36]2[CH:37]=[CH:38][C:33]([N:32]3[C:31](=[O:44])[C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[N:24]=[C:23]3[C:20]3[CH:21]=[N:22][C:17]([CH3:1])=[CH:18][CH:19]=3)=[CH:34][CH:35]=2)[CH2:40][CH2:41][CH2:42][CH2:43]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 574072TrimethylboroxineHCID 86659813HCID 86659813, 화합물

생성물 1

HCID 46842007HCID 46842007, 화합물수율 27.4%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매
HCID 31275
1,4-Dioxane
용매

실험 절차

6-chloro-3-pyridinecarboxaldehyde (0.177 g, 1.20 mmol) and CuCl2 (0.335 g, 2.40 mmol) were added to a solution of 2-amino-N-(4-cyclopentylphenyl)benzamide (0.350 g, 1.20 mmol) in EtOH (30 mL), and refluxed for 5 hours. The reaction mixture was concentrated in vacuo and the residue was dissolved in EtOAc. The organics were washed with H2O, then brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification by flash chromatography on silica gel, eluting with 15% to 60% EtOAc in heptane, afforded 2-(6-chloropyridin-3-yl)-3-(4-cyclopentylphenyl)quinazolin-4(3H)-one (0.260 g, 54%). Pd(PPh3)4 (0.150 g, 0.12 mmol), K2CO3 (0.270 g, 1.90 mmol), and trimethylboroxine (0.18 mL, 1.20 mmol) were added to a solution of 2-(6-chloropyridin-3-yl)-3-(4-cyclopentylphenyl)quinazolin-4(3H)-one (0.260 g, 0.65 mmol) in dioxane (15 mL) and heated to reflux temperature for 20 minutes. The reaction mixture was filtered through Celite®, washed with EtOAc. The filtrate was concentrated and purified by flash chromatography on silica gel, eluting with 30% to 100% EtOAc in heptane, to afford the title compound as a white solid (0.068 g, 27%). 1H-NMR (300 MHz, DMSO-d6): δ8.45 (s, 1H), 8.19 (d, J=7.4 Hz, 1H), 7.84-8.00 (m, 1H), 7.78 (d, J=7.9 Hz, 1H), 7.50-7.70 (m, 2H), 7.17-7.31 (m, 4H), 7.11 (d, J=8.0 Hz, 1H), 2.85-3.06 (m, 1H), 2.38 (s, 3H), 1.85-2.09 (m, 2H), 1.34-1.84 (m, 6H). MS (APCI) m/z: 382 (M+H)+.

후처리

  1. temperatureheated
  2. temperatureto reflux temperature for 20 minutes
  3. filtrationThe reaction mixture was filtered through Celite®
  4. washwashed with EtOAc
  5. concentrationThe filtrate was concentrated
  6. custompurified by flash chromatography on silica gel
  7. washeluting with 30% to 100% EtOAc in heptane

출처 및 근거

ORD 기록
ord-fa716506d39c404bb4c78bfb23f3c3b2
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952021B2

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