Sodium Carbonate → HCID 67281089, 화합물

HRID 1694711

반응식

HRID 1694711 반응식
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

참가 물질

7

반응물 4

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

생성물 1

HCID 67281089HCID 67281089, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 887Methanol용매2회

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-c914bdbf71e24bb585e2f0d95f4ed87d
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158820B2

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