Methylamine → HCID 59218213, compound

HRID 2246222Notes

Reaction equation

HRID 2246222 reaction equation
[F:1][C:2]([F:31])([F:30])[C:3]1[CH:4]=[C:5]([C:9]2[N:14]=[N:13][C:12]([N:15]3[CH2:20][CH2:19][N:18]([C:21]([O:23][CH2:24][C:25]([O:27]CC)=O)=[O:22])[CH2:17][CH2:16]3)=[CH:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1.[CH3:32][NH2:33]>O1CCCC1.ClCCl.CO>[F:31][C:2]([F:30])([F:1])[C:3]1[CH:4]=[C:5]([C:9]2[N:14]=[N:13][C:12]([N:15]3[CH2:16][CH2:17][N:18]([C:21]([O:23][CH2:24][C:25]([NH:33][CH3:32])=[O:27])=[O:22])[CH2:19][CH2:20]3)=[CH:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1

Participants

6

Reactant 2

HCID 6329MethylamineHCID 60209565HCID 60209565, compound

Product 1

HCID 59218213HCID 59218213, compound

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 6344DichloromethaneSolventHCID 8028TetrahydrofuranSolvent

Procedure

The procedure described in Example 1 (step 1.4.) is used. Starting with 0.66 g (1.51 mmol) of 2-(ethyloxy)-2-oxo-ethyl 4-{6-[3-(trifluoromethyl)phenyl]-3-pyridazinyl}-1-piperazinecarboxylate, obtained in step 10.2., and 3 ml (6.02 mmol) of a solution of methylamine (2M) in tetrahydrofuran, and after chromatography on silica gel, eluting with a 96/4 mixture of dichloromethane and methanol, followed by washing with diisopropyl ether, 0.50 g of product is obtained in the form of a white solid.

Workup

  1. customobtained in step 10.2
  2. washby washing with diisopropyl ether

Sources & evidence

ORD record
ord-8850ddd483a8444495ce6208eebea9a7
Source dataset
uspto-grants-2010_03
Patent number
US07687503B2

Reaction notes

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