Methylamine → HCID 69435629, compound

HRID 1297051Notes

Reaction equation

HRID 1297051 reaction equation
[CH3:1][NH2:2].[Br:3][C:4]1[C:8]([N+:9]([O-:11])=[O:10])=[C:7](Br)[N:6]([CH2:13][CH2:14][O:15][CH3:16])[N:5]=1>C(O)C>[Br:3][C:4]1[C:8]([N+:9]([O-:11])=[O:10])=[C:7]([NH:2][CH3:1])[N:6]([CH2:13][CH2:14][O:15][CH3:16])[N:5]=1

Participants

4

Conditions

Temperature
22.5 °C

Procedure

Aqueous 40% methylamine solution (300 ml, 8.71 mol) was added to a solution of 3,5-dibromo-1-(2′-methoxyethyl)4-nitropyrazole (15 g, 0.483 mol) in ethanol (300 ml). The reaction mixture was stirred at 20-25° C. for 2 hours and then cooled to 0-5° C. for 30 minutes. The precipitate formed was filtered off and washed with a cold mixture of water/ethanol (1/1, 30 ml). The final amine product was obtained in the form of a yellow solid (4.6 g, 36%) after drying under reduced pressure.

Workup

  1. temperaturecooled to 0-5° C. for 30 minutes
  2. customThe precipitate formed
  3. filtrationwas filtered off
  4. washwashed with a cold mixture of water/ethanol (1/1, 30 ml)

Sources & evidence

ORD record
ord-b1cd3017dc67482aad0bcb68093c5d13
Source dataset
uspto-grants-2007_07
Patent number
US07250063B2

Reaction notes

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