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Potassium Phosphate, Tribasic → HCID 89963353, compound

HRID 1843945
Notes
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Reaction equation

HRID 1843945 reaction equation
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:14][C:8]3[C:9](=[O:13])[NH:10][CH2:11][CH2:12][C:7]=3[C:6]=2[CH:15]=1.I[C:17]1[CH:18]=[N:19][CH:20]=[CH:21][C:22]=1[CH3:23].[O-]P([O-])([O-])=O.[K+].[K+].[K+].CN[C@@H]1CCCC[C@H]1NC>[Cu]I.O1CCOCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:14][C:8]3[C:9](=[O:13])[N:10]([C:17]4[CH:18]=[N:19][CH:20]=[CH:21][C:22]=4[CH3:23])[CH2:11][CH2:12][C:7]=3[C:6]=2[CH:15]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 4

HCID 62657Potassium Phosphate, TribasicHCID 2733821trans-N,N'-dimethyl-1,2-cyclohexanediamineHCID 144235133-Iodo-4-methylpyridineHCID 89964359HCID 89964359, compound

Product 1

HCID 89963353HCID 89963353, compoundYield 37.81%

Reagents, catalysts & solvents 2

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

Conditions

Temperature
120 °C

Procedure

6-Fluoro-3,4-dihydro-2H-benzo[4,5]thieno[2,3-c]pyridin-1-one (I-45e: 85 mg, 0.384 mmol) was reacted with 3-iodo-4-methyl-pyridine (101 mg, 0.461 mmol), K3PO4 (244 mg, 1.152 mmol), trans-N,N′-dimethyl-cyclohexane-1,2-diamine (16.3 mg, 0.115 mmol), CuI (7.2 mg, 0.038 mmol) and 1,4-dioxane (10 mL). The resulting mixture was refluxed at 120° C. overnight to afford the crude product. Purification by column chromatography on silica gel (2% methanol in chloroform) afforded 45 mg of the product (37.81% yield).

Workup

  1. customto afford the crude product
  2. customPurification by column chromatography on silica gel (2% methanol in chloroform)

Sources & evidence

ORD record
ord-63aaedf98b584b989da0aa6b5fc26901
Source dataset
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08946260B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes