Nitrogen → HCID 86624326, compound

HRID 1993709Notes

Reaction equation

HRID 1993709 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[C:6]([C:10]1[CH:11]=[C:12]([NH:22][C:23]([NH:25][C:26]2[CH:27]=[N:28][C:29]([N:32]3[CH2:37][CH2:36][N:35]([C:38](=[O:45])[CH2:39][CH:40]4[CH2:44][CH2:43][CH2:42][CH2:41]4)[CH2:34][CH2:33]3)=[CH:30][CH:31]=2)=[O:24])[N:13]([C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=2)[N:14]=1)([CH3:9])([CH3:8])[CH3:7].N#N>C(Cl)Cl.CO>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[C:6]([C:10]1[CH:11]=[C:12]([NH:22][C:23]([NH:25][C:26]2[CH:27]=[N:28][C:29]([N:32]3[CH2:37][CH2:36][N:35]([C:38](=[O:45])[CH2:39][CH:40]4[CH2:44][CH2:43][CH2:42][CH2:41]4)[CH2:34][CH2:33]3)=[CH:30][CH:31]=2)=[O:24])[N:13]([C:15]2[CH:16]=[CH:17][C:18]([CH3:21])=[CH:19][CH:20]=2)[N:14]=1)([CH3:9])([CH3:7])[CH3:8]

Participants

5

Reactant 3

HCID 947NitrogenHCID 6395Methanesulfonic AcidHCID 59134460HCID 59134460, compound

Product 1

HCID 86624326HCID 86624326, compound

Reagents, catalysts & solvents 1

HCID 21226129Dichloromethane methanolSolvent2×

Procedure

Add 0.10 mL of 1N solution of methanesulfonic acid in CH2Cl2/MeOH (95/5) to a stirred solution of 1-(5-tert-butyl-2-p-tolyl-2H-pyrazol-3-yl)-3-{6-[4-(2-cyclopentyl-acetyl)-piperazin-1-yl]-pyridin-3-yl}-urea in 2 mL of CH2Cl2/MeOH (95/5). Stir the mixture at room temperature for 20 minutes, and then evaporate solvents by N2 flushing. Triturate the salt with Et2O, filter and dry to give the title compound. MS(ES+): m/z=544 [M+H].

Workup

  1. customTriturate the salt with Et2O
  2. filtrationfilter
  3. customdry

Sources & evidence

ORD record
ord-6a64b5fc6c4f4bd1bda15dc04a67b0a1
Source dataset
uspto-grants-2010_01
Patent number
US07652015B2

Reaction notes

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