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Water → Methyl 2-chloro-4-fluoro-5-(pyridin-2-yl)benzoate

HRID 522144
ノート
印刷プレビュー

反応式

HRID 522144 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]([F:12])[C:9](B2OC(C)(C)C(C)(C)O2)=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].Br[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=1.C(=O)([O-])[O-].[K+].[K+].O>C1COCC1.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>[Cl:1][C:2]1[CH:11]=[C:10]([F:12])[C:9]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=2)=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]
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 4

HCID 962WaterHCID 79732-BromopyridineHCID 11430Potassium CarbonateHCID 467394354-Chloro-2-fluoro-5-(methoxycarbonyl)phenylboronic acid, pinacol ester

生成物 1

HCID 118497122Methyl 2-chloro-4-fluoro-5-(pyridin-2-yl)benzoate収率 67.1%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl 2-chloro-4-fluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (212 mmol) in THF (400 mL), was added 2-bromopyridine (33.4 g, 211 mmol), potassium carbonate (117 g, 848 mmol) and water (64 mL). The mixture was degassed with argon for 30 minutes. To this mixture was added tetrakis(triphenylphosphine)palladium (12.2 g, 10.6 mmol) and the mixture heated at reflux for 1.5 h. The mixture was cooled to room temperature and filtered through Celite, washing with EtOAc (1.2 L) and water (800 mL). The filtrate was diluted with saturated aqueous brine solution (200 mL) and the aqueous layer separated and extracted with EtOAc (600 mL). The combined organic layers were dried (MgSO4) and concentrated in vacuo. The residue was purified by column chromatography over silica gel, eluting with EtOAc:hexane (3:17 to 1:4) and concentrated in vacuo to a slurry, which was diluted with heptane (100 mL) and cooled to 0° C. The solid was collected by filtration to afford the title compound (37.6 g, 67%).

後処理

  1. customThe mixture was degassed with argon for 30 minutes
  2. temperaturethe mixture heated
  3. temperatureat reflux for 1.5 h
  4. filtrationfiltered through Celite
  5. washwashing with EtOAc (1.2 L) and water (800 mL)
  6. additionThe filtrate was diluted with saturated aqueous brine solution (200 mL)
  7. customthe aqueous layer separated
  8. extractionextracted with EtOAc (600 mL)
  9. dry with materialThe combined organic layers were dried (MgSO4)
  10. concentrationconcentrated in vacuo
  11. customThe residue was purified by column chromatography over silica gel
  12. washeluting with EtOAc:hexane (3:17 to 1:4)
  13. concentrationconcentrated in vacuo to a slurry, which
  14. additionwas diluted with heptane (100 mL)
  15. temperaturecooled to 0° C
  16. filtrationThe solid was collected by filtration

出典と根拠

ORDレコード
ord-16d79907aacb4068a201e86aa840e640
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09328096B2

反応ノート

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