Methylhydrazine → HCID 71224662, compound

HRID 2402941Notes

Reaction equation

HRID 2402941 reaction equation
[C:1]([C:4]1[C:9]([C:10]([O:12]CC)=O)=[CH:8][N:7]=[C:6]([S:15][CH3:16])[N:5]=1)(=O)[CH3:2].[CH3:17][NH:18][NH2:19]>C(O)CCC>[CH3:17][N:18]1[C:10](=[O:12])[C:9]2[CH:8]=[N:7][C:6]([S:15][CH3:16])=[N:5][C:4]=2[C:1]([CH3:2])=[N:19]1

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 71224338HCID 71224338, compound

Product 1

HCID 71224662HCID 71224662, compound

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

A solution of Example 1B (600 mg, 2.497 mmol) and methylhydrazine (0.131 mL, 2.497 mmol) in n-butanol (12.5 mL) was heated to 140° C. by microwave irradiation (Biotage Initiator) for 30 minutes. The reaction mixture was cooled to room temperature, whereupon a solid crystallized from the solution. The solid was filtered, washed with hexane, and air-dried to provide the title compound. MS ESI(+) m/z 223 [M+H]+.

Workup

  1. customcrystallized from the solution
  2. filtrationThe solid was filtered
  3. washwashed with hexane
  4. customair-dried

Sources & evidence

ORD record
ord-35b57062ab2843eab935348db385148c
Source dataset
uspto-grants-2014_08
Patent number
US08796289B2

Reaction notes

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