Methanol → HCID 131726736, compound

HRID 2250540Notes

Reaction equation

HRID 2250540 reaction equation
[CH3:1][C:2]([N+:7]([O-:9])=[O:8])([CH2:5][OH:6])[CH2:3][OH:4].[CH3:10][C:11]([N:13]([CH3:15])[CH3:14])=[O:12].CO>C1(C)C=CC=CC=1>[CH3:10][C:11]([N:13]([CH3:15])[CH3:14])=[O:12].[CH3:1][C:2]([N+:7]([O-:9])=[O:8])([CH2:5][OH:6])[CH2:3][OH:4]

Participants

5

Reactant 3

HCID 887MethanolHCID 64802-Methyl-2-nitro-1,3-propanediolHCID 31374Dimethylacetamide

Product 1

HCID 131726736HCID 131726736, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

NMPD (ANGUS lot ZD-06024; 13.57 g, 0.10 moles) was dissolved in aqueous DMA (40 wt. percent, 12.6 mL, 4.53 g, 0.10 moles) with stirring at room temperature under nitrogen. Within 30 minutes the solution became very turbid and darker yellow in color. After 5 days at room temperature the reaction mixture was a white, waxy solid. The product was slurried with methanol and toluene, then the solvents were removed by rotary evaporation. The yield of off-white DMA-NMPD was 15.4 g (95 percent). MP was 73-77° C. GC analysis showed 4 area percent of NMPD.

Workup

  1. waitAfter 5 days at room temperature the reaction mixture was
  2. customthe solvents were removed by rotary evaporation

Sources & evidence

ORD record
ord-07cd6a0c824b4b03b3581b8c852b6f80
Source dataset
uspto-grants-2008_01
Patent number
US07317063B2

Reaction notes

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