Hydroxylamine → HCID 73734374, compound

HRID 1796653Notes

Reaction equation

HRID 1796653 reaction equation
[CH:1]([C:3]1[C:4]([CH3:28])=[C:5]2[C:10]([NH:11][C:12]3[CH:17]=[CH:16][C:15]([O:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)=[CH:14][CH:13]=3)=[C:9]([C:25]#[N:26])[CH:8]=[N:7][N:6]2[CH:27]=1)=O.[NH2:29][OH:30]>CO.O>[OH:30][N:29]=[CH:1][C:3]1[C:4]([CH3:28])=[C:5]2[C:10]([NH:11][C:12]3[CH:17]=[CH:16][C:15]([O:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)=[CH:14][CH:13]=3)=[C:9]([C:25]#[N:26])[CH:8]=[N:7][N:6]2[CH:27]=1

Participants

5

Reactant 2

HCID 787HydroxylamineHCID 22179494HCID 22179494, compound

Product 1

HCID 73734374HCID 73734374, compoundYield 78.2%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

To a slurry of 6-formyl-5-methyl-4-(4-phenoxy-phenylamino)-pyrrolo[1,2-b]pyridazine-3-carbonitrile (Example 8) (37 mg, 0.1 mmol) in MeOH (1 ml) was added H2NOH (50% wt. in H2O, 14 μl 0.2 mmol) at rt. The heterogeneous mixture was stirred overnight, then diluted with H2O (5 ml) and filtered, the solid was dissolved in MeOH, which was concentrated to give title compound (30 mg, 78%) as a yellow powder. It has a retention time of 6.18 min (standard LCl method, 8 min run). MS Found: (M+H)+=384.2

Workup

  1. filtrationfiltered
  2. dissolutionthe solid was dissolved in MeOH
  3. concentrationwhich was concentrated

Sources & evidence

ORD record
ord-c9e2402827c549dcb1566c1ff8976be6
Source dataset
uspto-grants-2006_04
Patent number
US07030112B2

Reaction notes

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