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Potassium Carbonate → HCID 89924531, 화합물

HRID 1505671
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HRID 1505671 반응식
Br[C:2]1[CH:3]=[N:4][C:5]([C:8]2[CH:9]=[C:10]([CH:12]=[CH:13][CH:14]=2)[NH2:11])=[N:6][CH:7]=1.B(O)(O)[C:16]1[CH:20]=[N:19][N:18]([CH:21]2[CH2:26][CH2:25][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:23][CH2:22]2)[CH:17]=1.C([O-])([O-])=O.[K+].[K+]>O1CCOCC1.O.CCOC(C)=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>[NH2:11][C:10]1[CH:9]=[C:8]([C:5]2[N:4]=[CH:3][C:2]([C:16]3[CH:20]=[N:19][N:18]([CH:21]4[CH2:22][CH2:23][N:24]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:25][CH2:26]4)[CH:17]=3)=[CH:7][N:6]=2)[CH:14]=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 46739790(1-(1-(tert-Butoxycarbonyl)piperidin-4-yl)-1H-pyrazol-4-yl)boronic acidHCID 63318778HCID 63318778, 화합물2회

생성물 1

HCID 89924531HCID 89924531, 화합물

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매
HCID 8857
Ethyl Acetate
용매
HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

A mixture of 3-(5-bromopyrimidin-2-yl)aniline (intermediate 4, 220 mg; 0.88 mmol; 1.0 eq.), 1-(1-Boc-piperidino)pyrazole-4-boronic acid (389 mg; 1.3 mmol; 1.5 eq.), Pd(PPh3)4 (51 mg; 0.04 mmol; 0.05 eq.) and K2CO3 (365 mg; 2.6 mmol; 3.0 eq.) in dioxane/water (3.3: 1.65 mL) was heated at 12000 for 30 min in a sealed tube in MW. The reaction mixture was then diluted with EtOAc. The two phases were separated and aqueous phase was extracted with EtOAc. Combined organic phases were dried over magnesium sulfate, filtered and concentrated. Flash chromatography on silica (EtOAc:heptane, gradient from 50:50 to 100:0) afforded the title compound a beige solid (240 mg; 65%). 1H NMR (300 MHz, DMSO-d6) δ 9.09 (s, 2H), 8.52 (s, 1H), 8.11 (s, 1H), 7.67 (t, J=2.0 Hz, 1H), 7.57-7.53 (m, 1H), 7.14 (t, J=7.8 Hz, 1H), 6.69-6.66 (m, 1H), 5.25 (s, 2H), 4.46-4.36 (m, 1H), 4.08-4.04 (m, 2H), 2.94 (m, 2H), 2.08-2.04 (m, 2H), 1.87-1.75 (m, 2H), 1.43 (s, 9H). HPLC (Condition A): Rt 3.03 min (purity 99.0%). MS (ESI+): 421.4.

후처리

  1. temperaturewas heated at 12000 for 30 min in a sealed tube in MW
  2. customThe two phases were separated
  3. extractionaqueous phase was extracted with EtOAc
  4. dry with materialCombined organic phases were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0f1447481c8f46baba40f93663df25e0
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216991B2

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