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

HRID 1091620
ノート
印刷プレビュー

反応式

HRID 1091620 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-02e3e27bfd314caf858b446cbf46b182
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129394B2

反応ノート

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