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Sodium Carbonate → 2-(2-Fluoro-6-methoxy-phenyl)-thiazole-4-carboxylic acid

HRID 1990993
ノート
印刷プレビュー

反応式

HRID 1990993 の反応式
C([O:3][C:4]([C:6]1[N:7]=[C:8](Br)[S:9][CH:10]=1)=[O:5])C.CO[C:14]1(B(O)O)[C:19]([F:20])=[CH:18][CH:17]=[CH:16][CH2:15]1.[C:24](=[O:27])([O-])[O-].[Na+].[Na+]>COCCOC.CN(C=O)C.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:20][C:19]1[CH:14]=[CH:15][CH:16]=[C:17]([O:27][CH3:24])[C:18]=1[C:8]1[S:9][CH:10]=[C:6]([C:4]([OH:3])=[O:5])[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 10340Sodium CarbonateHCID 353965Ethyl 2-bromo-1,3-thiazole-4-carboxylateHCID 866136741-Methoxy-6-flurophenylboronic acid

生成物 1

HCID 589248452-(2-Fluoro-6-methoxy-phenyl)-thiazole-4-carboxylic acid

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒
HCID 6228
Dimethylformamide
溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

Tetrakis(triphenylphosphine)palladium (0.54 g, 0.48 mmol, 2.2% mol eq) was added to a degassed (nitrogen) mixture of 2-bromo-thiazole-4-carboxylic acid ethyl ester (Combi-Blocks, Inc., San Diego, Calif.; 5 g, 21.2 mmol), 1-methoxy-6-flurophenylboronic acid (4.68 g, 27.56 mmol), and sodium carbonate(23 mL, 2 M solution in water) in DME (100 mL) and DMF (100 mL). The reaction mixture was refluxed under inert atmosphere overnight. After cooling to room temperature, the reaction mixture was filtered through celite, and water and EtOAc were added. The aqueous layer was separated, acidified with conc. HCl to pH 2 and then was extracted three times with EtOAc. The combined EtOAc layers were dried under vacuum. The residue was chromatographed on silica, eluting with EtOAc/Hexane (0-30% gradient) to give 2-(2-fluoro-6-methoxy-phenyl)-thiazole-4-carboxylic acid (4.5 g) which was used directly in the next step.

後処理

  1. customa degassed
  2. temperatureThe reaction mixture was refluxed under inert atmosphere overnight
  3. filtrationthe reaction mixture was filtered through celite, and water and EtOAc
  4. additionwere added
  5. customThe aqueous layer was separated
  6. extractionwas extracted three times with EtOAc
  7. dry with materialThe combined EtOAc layers were dried under vacuum
  8. customThe residue was chromatographed on silica
  9. washeluting with EtOAc/Hexane (0-30% gradient)

出典と根拠

ORDレコード
ord-08e6939888104eaba9be008a42dc1356
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07645773B2

反応ノート

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