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Cesium fluoride → 5-(2-Chlorophenylthio)-6-(4-methylthiazol-2-ylamino)pyridin-3-ol

HRID 1806027
ノート
印刷プレビュー

反応式

HRID 1806027 の反応式
Br[C:2]1[CH:3]=[C:4]([S:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[Cl:22])[C:5]([NH:8][C:9]2[S:10][CH:11]=[C:12]([CH3:14])[N:13]=2)=[N:6][CH:7]=1.CC1(C)C(C)(C)OB(B2OC(C)(C)C(C)(C)O2)[O:25]1.C1(P(C2CCCC2)C2CCCC2)CCCC1.[F-].[Cs+]>C(#N)C.CC([O-])=O.CC([O-])=O.[Pd+2]>[Cl:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[S:15][C:4]1[CH:3]=[C:2]([OH:25])[CH:7]=[N:6][C:5]=1[NH:8][C:9]1[S:10][CH:11]=[C:12]([CH3:14])[N:13]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 25953Cesium fluorideHCID 2733548Bis(pinacolato)diboraneHCID 4463278Phosphine, tricyclopentyl-HCID 24764526N-(5-bromo-3-(2-chlorophenylthio)pyridin-2-yl)-4-methylthiazol-2-amine

生成物 1

HCID 247645195-(2-Chlorophenylthio)-6-(4-methylthiazol-2-ylamino)pyridin-3-ol

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
HCID 6342Acetonitrile溶媒

反応条件

温度
90 °C

実験手順

A degassed mixture of N-(5-bromo-3-(2-chlorophenylthio)pyridin-2-yl)-4-methylthiazol-2-amine (1.10 g, 2.66 mmol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (1.35 g, 5.32 mmol), Pd(OAc)2 (60 mg, 0.27 mmol), tricyclopentylphosphine (93 mg. 0.40 mmol) and cesium fluoride (3.64 g, 23.9 mmol) in acetonitrile is heated at 90° C. for 5 hours. The reaction mixture is cooled and partitioned between ether and water. The crude product is dissolved in THF. N-morpholine N-oxide (1.40 g, 12.0 mmol) is added and the reaction mixture is heated at reflux for 12 hours. The reaction mixture is cooled and partitioned between ether and water. The organic layer is washed with water and brine, dried and concentrated. The residue is purified by silica gel chromatography, eluting with 10-20% EtOAc in hexanes to afford the title compound.

後処理

  1. temperatureThe reaction mixture is cooled
  2. custompartitioned between ether and water
  3. dissolutionThe crude product is dissolved in THF
  4. temperaturethe reaction mixture is heated
  5. temperatureat reflux for 12 hours
  6. temperatureThe reaction mixture is cooled
  7. custompartitioned between ether and water
  8. washThe organic layer is washed with water and brine
  9. customdried
  10. concentrationconcentrated
  11. customThe residue is purified by silica gel chromatography
  12. washeluting with 10-20% EtOAc in hexanes

出典と根拠

ORDレコード
ord-4be61383afca4b9dbda5ac66457c36b4
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08354540B2

反応ノート

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