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Sodium Carbonate → N-[4-(5-formyl-4-phenyl-1,3-thiazol-2-yl)pyridin-2-yl]acetamide

HRID 1530133
ノート
印刷プレビュー

反応式

HRID 1530133 の反応式
F[B-](F)(F)F.C([PH+](C(C)(C)C)C(C)(C)C)(C)(C)C.C(=O)([O-])[O-].[Na+].[Na+].[C:25]1(B(O)O)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.Cl[C:35]1[N:36]=[C:37]([C:42]2[CH:47]=[CH:46][N:45]=[C:44]([NH:48][C:49](=[O:51])[CH3:50])[CH:43]=2)[S:38][C:39]=1[CH:40]=[O:41]>COCCOC.O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH:40]([C:39]1[S:38][C:37]([C:42]2[CH:47]=[CH:46][N:45]=[C:44]([NH:48][C:49](=[O:51])[CH3:50])[CH:43]=2)=[N:36][C:35]=1[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:41]
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

8

反応物 4

HCID 10340Sodium CarbonateHCID 66827Phenylboronic AcidHCID 2734635Tri-tert-butylphosphine tetrafluoroborateHCID 86649613N-[4-(4-chloro-5-formyl-1,3-thiazol-2-yl)pyridin-2-yl]acetamide

生成物 1

HCID 86649614N-[4-(5-formyl-4-phenyl-1,3-thiazol-2-yl)pyridin-2-yl]acetamide収率 43.1%

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒2 回
HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
80 °C

実験手順

Tris(dibenzylideneacetone)dipalladium(0) (0.0162 g, 0.0177 mmol) and tri-t-butylphosphonium tetrafluoroborate (0.0103 g, 0.0355 mmol) were weighed into a round bottom flask and dissolved in DME (3 mL). The mixture was sonicated for 15 min under atmosphere of Argon. After addition of water (1 mL), sodium carbonate (0.226 g, 2.13 mmol) was added to the dark purple solution followed by phenylboronic acid (0.173 g, 1.42 mmol) and N-[4-(4-chloro-5-formyl-1,3-thiazol-2-yl)pyridin-2-yl]acetamide (0.200 g, 0.710 mmol). The resulting mixture was stirred for 10 h at 80° C., cooled to room temperature, diluted with water and extracted with DCM (3×5 mL). The organics were washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated. The result mixture was purified by ISCO column with 0-5% MeOH in DCM in 10 min. Fractions containing product were combined and solvent was removed under reduced pressure to give crude material (0.099 g, 43%), which was used in the next step without further purification. LCMS: (FA) ES+ 324.

後処理

  1. customThe mixture was sonicated for 15 min under atmosphere of Argon
  2. additionwas added to the dark purple solution
  3. temperaturecooled to room temperature
  4. extractionextracted with DCM (3×5 mL)
  5. washThe organics were washed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe result mixture was purified by ISCO column with 0-5% MeOH in DCM in 10 min
  10. additionFractions containing product
  11. customsolvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-5971a74d3bd84e3bbc554392faaac069
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090601B2

反応ノート

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