Methylhydrazine → HCID 68690143, compound

HRID 1172842Notes

Reaction equation

HRID 1172842 reaction equation
[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][C:5]([C:10]([C:12]2[C:13]([CH2:26][CH2:27][CH3:28])=[N:14][CH:15]=[CH:16][C:17]=2OC2C=CC(Cl)=CC=2)=O)=[C:4](F)[CH:3]=1.[CH3:30][NH:31][NH2:32].C([O:36][CH2:37][CH3:38])(=O)C>CS(C)=O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:5]([C:10]([C:12]3[C:13]([CH2:26][CH2:27][CH3:28])=[N:14][C:15]([O:36][C:37]4[CH:38]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=4)=[CH:16][CH:17]=3)=[N:32][N:31]2[CH3:30])=[CH:6][C:7]=1[O:8][CH3:9]

Participants

5

Reactant 3

HCID 6061MethylhydrazineHCID 8857Ethyl AcetateHCID 68696356HCID 68696356, compound

Product 1

HCID 68690143HCID 68690143, compound

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent

Procedure

A solution of the ketone from Step 7 of Example 12 (0.86 g, 2.0 mmol) and methylhydrazine (0.18 g, 4.0 mmol) in DMSO (10 mL) was heated at 80° C. for 1 h. The mixture was diluted with ethyl acetate, washed with water and dried over magnesium sulfate. After removal of the solvent, the residue was purified by chromatography on silica gel to give the title product.

Workup

  1. washwashed with water
  2. dry with materialdried over magnesium sulfate
  3. customAfter removal of the solvent
  4. customthe residue was purified by chromatography on silica gel

Sources & evidence

ORD record
ord-e42dec222b2a469d85e3edbc494aee14
Source dataset
uspto-grants-2010_11
Patent number
US07834036B2

Reaction notes

Loading…