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Sodium Methoxide → methyl 4-iodo-1H-pyrrole-2-carboxylate

HRID 384414
Notes
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Reaction equation

HRID 384414 reaction equation
ClC(Cl)(Cl)[C:3]([C:5]1[NH:6][CH:7]=[C:8]([I:10])[CH:9]=1)=[O:4].[CH3:13][O-:14].[Na+]>CO>[CH3:13][O:14][C:3]([C:5]1[NH:6][CH:7]=[C:8]([I:10])[CH:9]=1)=[O:4]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 10942334Sodium MethoxideHCID 116816022,2,2-trichloro-1-(4-iodo-1H-pyrrol-2-yl)ethan-1-one

Product 1

HCID 11673249methyl 4-iodo-1H-pyrrole-2-carboxylateYield 94.3%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

2,2,2-Trichloro-1-(4-iodo-1H-pyrrol-2-yl)-ethanone 57c (47 g, 136 mmol) was dissolved in 265 mL of methanol followed by dropwise addition of a solution of sodium methoxide (17.23 g, 163 mmol) in 200 mL of methanol. The reaction mixture was stirred at room temperature for 1 hour. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was concentrated under reduced pressure. The residue was diluted with 20 mL of water and then extracted with ethyl acetate (30 mL×3). The combined organic extracts were washed with saturated brine, dried over anhydrous sodium sulfate, filtered to remove the drying agent and concentrated under reduced pressure to obtain the title compound 4-iodo-1H-pyrrole-2-carboxylic acid methyl ester 57d (32.2 g, yield 92.5%) as a grey solid.

Workup

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additionThe residue was diluted with 20 mL of water
  3. extractionextracted with ethyl acetate (30 mL×3)
  4. washThe combined organic extracts were washed with saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customto remove the drying agent
  8. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-7e4ccba829bf4dabaead2a78dbccec1e
Source dataset
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08367710B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes