Sodium Carbonate → HCID 67281089、化合物

HRID 1694711

反応式

HRID 1694711 の反応式
C1(C)C=CC(P(C2C=CC(C)=CC=2)C2C=CC(C)=CC=2)=CC=1.[OH:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]([F:33])([F:32])[F:31])=[CH:26][C:25]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+].[Cl:43][C:44]1[CH:49]=[C:48]([S:50][CH2:51][CH3:52])[CH:47]=[CH:46][C:45]=1I>CO.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:43][C:44]1[CH:49]=[C:48]([S:50][CH2:51][CH3:52])[CH:47]=[CH:46][C:45]=1[C:25]1[C:24]([OH:23])=[CH:29][CH:28]=[C:27]([C:30]([F:33])([F:32])[F:31])[CH:26]=1

参加物

7

反応物 4

HCID 10340Sodium CarbonateHCID 13956Phosphine, tris(4-methylphenyl)-HCID 59436609(2-Hydroxy-5-(trifluoromethyl)phenyl)boronic acidHCID 672801852-Chloro-4-(ethylthio)-1-iodo-benzene

生成物 1

HCID 67281089HCID 67281089、化合物

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 887Methanol溶媒2 回

実験手順

A mixture of palladium acetate (0.045 g) and tri-p-tolylphosphine (0.213 g) in methanol (10 ml) was stirred at RT for 30 min. The product from step (iii) (1 g), sodium carbonate (1.27 g), the product from example (26) step (i) (1.19 g) and methanol (20 ml) were added and the mixture heated under reflux for 6 h. The solvent was removed under reduced pressure and the residue partitioned between diethylether and 2M hydrochloric acid. The organics were separated, dried and evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with 10% ethylacetate/isohexane. Yield 0.503 g

後処理

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 6 h
  3. customThe solvent was removed under reduced pressure
  4. customthe residue partitioned between diethylether and 2M hydrochloric acid
  5. customThe organics were separated
  6. customdried
  7. customevaporated under reduced pressure
  8. customThe residue was purified by chromatography on silica eluting with 10% ethylacetate/isohexane

出典と根拠

ORDレコード
ord-c914bdbf71e24bb585e2f0d95f4ed87d
出典データセット
uspto-grants-2012_04
特許番号
US08158820B2

関連ノート

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