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Sodium Carbonate → 5-(2-(4-Fluorophenyl)-5-(pyridin-4-yl)thiazol-4-yl)-3-methoxypyridin-2-amine

HRID 538429
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HRID 538429 반응식
Br[C:2]1[S:6][C:5]([C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)=[N:4][C:3]=1[C:14]1[CH:15]=[C:16]([O:21][CH3:22])[C:17]([NH2:20])=[N:18][CH:19]=1.[N:23]1[CH:28]=[CH:27][C:26](B(O)O)=[CH:25][CH:24]=1.C([O-])([O-])=O.[Na+].[Na+]>COCCOC.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>[F:13][C:10]1[CH:11]=[CH:12][C:7]([C:5]2[S:6][C:2]([C:26]3[CH:27]=[CH:28][N:23]=[CH:24][CH:25]=3)=[C:3]([C:14]3[CH:15]=[C:16]([O:21][CH3:22])[C:17]([NH2:20])=[N:18][CH:19]=3)[N:4]=2)=[CH:8][CH:9]=1
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참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 2734379(Pyridin-4-yl)boronic acidHCID 665911925-(5-Bromo-2-(4-fluorophenyl)thiazol-4-yl)-3-methoxypyridin-2-amine

생성물 1

HCID 591375455-(2-(4-Fluorophenyl)-5-(pyridin-4-yl)thiazol-4-yl)-3-methoxypyridin-2-amine수율 55.3%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 80711,2-Dimethoxyethane용매

실험 절차

A mixture of 5-(5-bromo-2-(4-fluorophenyl)thiazol-4-yl)-3-methoxypyridin-2-amine (40 mg, 0.11 mmol), 4-pyridineboronic acid (39 mg, 0.32 mmol), and, and aqueous 2.0 M Na2CO3 solution (0.6 mL) in DME (1.8 mL) was sparged with Ar for 3 min. Tetrakis(triphenylphosphine)palladium(0) (20 mg, 0.02 mmol) was added and the reaction mixture was sparged with Ar for 1 min. The reaction was sealed and irradiated at 115° C. for 15 min in a microwave reactor. The reaction mixture was partitioned with EtOAc (25 mL) and saturated aqueous NaHCO3 solution (25 mL). The separated organic layer was washed with saturated aqueous NaHCO3 solution (25 mL), brine (25 mL), dried (Na2SO4), filtered and concentrated in vacuo. The resulting residue was purified by reverse phase HPLC, which after lypholization, provided 23 mg of the titled compound as the TFA salt: LCMS (m/z): 378.9 (MH+), tR=0.57 min.

후처리

  1. customwas sparged with Ar for 3 min
  2. customthe reaction mixture was sparged with Ar for 1 min
  3. customThe reaction was sealed
  4. customirradiated at 115° C. for 15 min in a microwave reactor
  5. customThe reaction mixture was partitioned with EtOAc (25 mL) and saturated aqueous NaHCO3 solution (25 mL)
  6. washThe separated organic layer was washed with saturated aqueous NaHCO3 solution (25 mL), brine (25 mL)
  7. dry with materialdried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe resulting residue was purified by reverse phase HPLC, which after lypholization

출처 및 근거

ORD 기록
ord-a52a1bddcff04ce0bf276e87a217d61d
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865732B2

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