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Potassium Carbonate → 3-(4-Fluoro-3-(methylsulfonyl)phenyl)-4-methoxybenzaldehyde

HRID 68608
Notes
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Reaction equation

HRID 68608 reaction equation
[CH:1]([C:3]1[CH:4]=[CH:5][C:6]([O:12][CH3:13])=[C:7](B(O)O)[CH:8]=1)=[O:2].Br[C:15]1[CH:20]=[CH:19][C:18]([F:21])=[C:17]([S:22]([CH3:25])(=[O:24])=[O:23])[CH:16]=1.C([O-])([O-])=O.[K+].[K+]>O1CCOCC1.O.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:21][C:18]1[CH:19]=[CH:20][C:15]([C:7]2[CH:8]=[C:3]([CH:4]=[CH:5][C:6]=2[O:12][CH3:13])[CH:1]=[O:2])=[CH:16][C:17]=1[S:22]([CH3:25])(=[O:23])=[O:24]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 3

HCID 11430Potassium CarbonateHCID 27343675-Formyl-2-methoxyphenylboronic acidHCID 269854244-Bromo-1-fluoro-2-(methylsulphonyl)benzene

Product 1

HCID 866818393-(4-Fluoro-3-(methylsulfonyl)phenyl)-4-methoxybenzaldehydeYield 108.1%

Reagents, catalysts & solvents 2

HCID 178418397
HCID 178418397, compound
Catalyst
HCID 218864351,4-Dioxane--water (1/1)Solvent

Conditions

Temperature
140 °C

Procedure

To a solution of 5-Formyl-2-methoxyphenylboronic acid (324 mg, 1.8 mmol, 1.5 eq, Frontier Scientific, Inc., Logan, Utah, USA) in dioxane:H2O (2:1; 15 mL) was added 4-bromo-1-fluoro-2-(methylsulfonyl)benzene (300 mg, 1.2 mmol, 1.0 eq., Apollo Scientific Ltd., Stockport, Cheshire, UK), K2CO3 (496 mg, 3.6 mmol, 2 eq.) and Pd(PPh3)4 (30 mg). The mixture was stirred under nitrogen at 140° C. in a microwave for 40 min. Solvent was evaporated and the residue was dissolved in DCM and washed with water. The DCM layer was dried and evaporated. Purification via column chromatography (eluent: PE:EA=3:1) yielded 400 mg (72%) of 3-(4-fluoro-3-(methylsulfonyl)phenyl)-4-methoxybenzaldehyde (27).

Workup

  1. customSolvent was evaporated
  2. dissolutionthe residue was dissolved in DCM
  3. washwashed with water
  4. dry with materialThe DCM layer was dried
  5. customevaporated
  6. customPurification via column chromatography (eluent: PE:EA=3:1)

Sources & evidence

ORD record
ord-45f4597c36274a5b985838bc77ac4440
Source dataset
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08822467B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes