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Lithium Chloride → HCID 66749451, compound

HRID 537042
Notes
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Reaction equation

HRID 537042 reaction equation
I[C:2]1[O:3][C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:5]([I:7])[N:6]=1.[CH3:13][C:14]1[C:15]([Sn](C)(C)C)=[CH:16][C:17]([NH:20][C:21](=[O:23])[CH3:22])=[N:18][CH:19]=1.[Cl-].[Li+]>O1CCOCC1.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.[Cu]I>[C:21]([NH:20][C:17]1[CH:16]=[C:15]([C:2]2[O:3][C:4]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:5]([I:7])[N:6]=2)[C:14]([CH3:13])=[CH:19][N:18]=1)(=[O:23])[CH3:22]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 3

HCID 433294Lithium ChlorideHCID 10596718HCID 10596718, compoundHCID 66747865HCID 66747865, compound

Product 1

HCID 66749451HCID 66749451, compoundYield 42%

Reagents, catalysts & solvents 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)Catalyst
HCID 178418397
HCID 178418397, compound
Catalyst
HCID 312751,4-DioxaneSolvent

Conditions

Temperature
100 °C

Procedure

A mixture of ethyl 2,4-diiodo-1,3-oxazole-5-carboxylate (0.37 g, 0.93 mmol), N-[5-methyl-4-(trimethylstannyl)pyridine-2-yl]acetamide (0.32 g, 1.0 mmol), tetrakis(triphenylphosphine)palladium(0) (0.054 g, 0.047 mmol), copper(I) iodide (0.053 g, 0.28 mmol) and lithium chloride (0.12 g, 2.8 mmol) in 1,4-dioxane (9 mL) was degassed with argon three times. The mixture was allowed to stir at 100° C. for 2 h under an atmosphere of argon and was then filtered while hot. The reaction mixture was concentrated and the residue was purified by column chromatography to give ethyl 2-[2-(acetylamino)-5-methylpyridin-4-yl]-4-iodo-1,3-oxazole-5-carboxylate (0.16 g, 42%).

Workup

  1. customwas degassed with argon three times
  2. filtrationwas then filtered while hot
  3. concentrationThe reaction mixture was concentrated
  4. customthe residue was purified by column chromatography

Sources & evidence

ORD record
ord-a8d8a488172f493caadb88407a0825ad
Source dataset
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08859768B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes