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Potassium Carbonate → 5-(5-chloropyridazin-3-yl)-1-methyl-1H-indazole

HRID 879396
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HRID 879396 반응식
Cl[C:2]1[N:3]=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.[CH3:9][N:10]1[C:18]2[C:13](=[CH:14][C:15](B(O)O)=[CH:16][CH:17]=2)[CH:12]=[N:11]1.C([O-])([O-])=O.[K+].[K+]>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>[Cl:8][C:6]1[CH:7]=[C:2]([C:15]2[CH:14]=[C:13]3[C:18](=[CH:17][CH:16]=2)[N:10]([CH3:9])[N:11]=[CH:12]3)[N:3]=[N:4][CH:5]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 199596873,5-DichloropyridazineHCID 225589101-Methyl-1H-indazole-5-boronic acid

생성물 1

HCID 867002035-(5-chloropyridazin-3-yl)-1-methyl-1H-indazole

시약·촉매·용매 1

HCID 178418397HCID 178418397, 화합물촉매

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온도
95 °C

실험 절차

3,5-dichloropyridazine (200 mg, 1.34 mmol), 1-methyl-1H-indazole-5-boronic acid (260 mg, 1.48 mmol), K2CO3 (556.6 mg, 4.03 mmol), and tetrakis(triphenylphosphine)palladium(0) (233, 0.20 mmol) were taken in a microwave vial, and the vial was vacuum pumped and flushed with argon three times. To this mixture was added degassed 1,4-dioxane (10 mL) and degassed water (2.5 mL). The reaction mixture was heated at 95° C. for 2 h then cooled to room temperature. The reaction mixture was filtered through Celite (ethyl acetate eluent) and concentrated. Purification by flash column chromatography on silica gel (hexanes/ethyl acetate eluent) provided the product. LCMS-ESI+: calc'd for C14H10ClN4: 245.1 (M+H+); Found: 245.2 (M+H+). 1H NMR (400 MHz, Chloroform-d) δ 9.15 (d, J=2.2 Hz, 1H), 8.44 (s, 1H), 8.21 (dd, J=8.8, 1.5 Hz, 1H), 8.11 (s, 1H), 7.97 (s, 1H), 7.56 (d, J=8.8 Hz, 1H), 4.14 (s, 3H).

후처리

  1. customflushed with argon three times
  2. additionTo this mixture was added
  3. customdegassed 1,4-dioxane (10 mL)
  4. customdegassed water (2.5 mL)
  5. temperaturethen cooled to room temperature
  6. filtrationThe reaction mixture was filtered through Celite (ethyl acetate eluent)
  7. concentrationconcentrated
  8. customPurification by flash column chromatography on silica gel (hexanes/ethyl acetate eluent)
  9. customprovided the product

출처 및 근거

ORD 기록
ord-93210446a980437181a609f7022fb7f9
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987250B2

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