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Dimethylformamide → HCID 178457084, compound

HRID 559613
Notes
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Reaction equation

HRID 559613 reaction equation
C([O:8][C:9]1[CH:17]=[C:16]([O:18]CC2C=CC=CC=2)[C:15]([CH:26]([CH3:28])[CH3:27])=[CH:14][C:10]=1[C:11](O)=O)C1C=CC=CC=1.C(Cl)(=O)C(Cl)=O.C[N:36]([CH:38]=[O:39])C.[CH3:40][O:41][C:42]1[CH:47]=[CH:46][C:45]([NH2:48])=[CH:44][C:43]=1[N:49]([CH3:53])[CH2:50][CH2:51][CH3:52].C([N:56](CC)CC)C>ClCCl.C1COCC1.O.C(OCC)(=O)C>[OH:39][C:38]1[N:48]([C:45]2[CH:46]=[CH:47][C:42]([O:41][CH3:40])=[C:43]([N:49]([CH3:53])[CH2:50][CH2:51][CH3:52])[CH:44]=2)[C:11]([C:10]2[CH:14]=[C:15]([CH:26]([CH3:27])[CH3:28])[C:16]([OH:18])=[CH:17][C:9]=2[OH:8])=[N:56][N:36]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

10

Reactant 5

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 591678792,4-Dibenzyloxy-5-isopropyl-benzoic acidHCID 591678804-Methoxy-N3-methyl-N3-propyl-benzene-1,3-diamine

Product 1

HCID 178457084HCID 178457084, compound
Yield 93%

Reagents, catalysts & solvents 4

HCID 962WaterSolventHCID 6344DichloromethaneSolventHCID 8028TetrahydrofuranSolvent2×HCID 8857Ethyl AcetateSolvent

Procedure

2,4-Bis-benzyloxy-5-isopropylbenzoic acid (1.25 g, 3.32 mmol) was dissolved in dichloromethane (50 mL) and cooled in an ice bath. Oxalyl chloride (0.32 mL, 3.65 mmol) was added followed by the dropwise addition of DMF (0.1 mL). The reaction was stirred at room temperature for 1 hr then evaporated to dryness under reduced pressure to produce a brown solid. This solid was dissolved in THF (50 mL) and cooled in an ice bath. A solution of 4-Methoxy-N3-methyl-N3-propyl-benzene-1,3-diamine (0.71 g, 3.65 mmol) in THF (20 mL) was added dropwisely followed by the triethylamine (1.6 mL) and the reaction was stirred at room temperature for 16 hrs. Ethyl acetate (50 mL) and water (100 mL) were added. The ethyl acetate layer was washed with water (3×50 mL), dried over magnesium sulfate, filtered and evaporated to dryness to produce the crude product as a brown solid. Purification by silicagel chromatography (elution with 25% ethyl acetate/hexane) provided the desired compound as a white solid (1.8 g, 93%).

Workup

  1. temperaturecooled in an ice bath
  2. customthen evaporated to dryness under reduced pressure
  3. customto produce a brown solid
  4. temperaturecooled in an ice bath
  5. stirringthe reaction was stirred at room temperature for 16 hrs
  6. washThe ethyl acetate layer was washed with water (3×50 mL)
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customevaporated to dryness
  10. customto produce the crude product as a brown solid
  11. customPurification
  12. washby silicagel chromatography (elution with 25% ethyl acetate/hexane)

Sources & evidence

ORD record
ord-b3c66624913945769ce58e1600c530f1
Source dataset
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08063083B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes