Water → HCID 131730215, compound

HRID 388508Notes

Reaction equation

HRID 388508 reaction equation
[F:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([N:18]3[CH2:23][CH2:22][CH:21]([N:24]4[CH2:29][CH2:28][N:27]([CH3:30])[CH2:26][CH2:25]4)[CH2:20][CH2:19]3)=[O:17])[CH:10]=2)[CH:5]=[CH:4][C:3]=1[NH:31][C:32]([CH2:34][C:35]1([CH2:38][C:39]([NH:41][C:42]2[CH:47]=[CH:46][C:45]([F:48])=[CH:44][CH:43]=2)=[O:40])[CH2:37][CH2:36]1)=[O:33].O.[S:50](=[O:54])(=[O:53])([OH:52])[OH:51]>C(O)C>[S:50]([OH:54])([OH:53])(=[O:52])=[O:51].[F:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]([N:18]3[CH2:19][CH2:20][CH:21]([N:24]4[CH2:29][CH2:28][N:27]([CH3:30])[CH2:26][CH2:25]4)[CH2:22][CH2:23]3)=[O:17])[CH:10]=2)[CH:5]=[CH:4][C:3]=1[NH:31][C:32]([CH2:34][C:35]1([CH2:38][C:39]([NH:41][C:42]2[CH:47]=[CH:46][C:45]([F:48])=[CH:44][CH:43]=2)=[O:40])[CH2:37][CH2:36]1)=[O:33]

Participants

5

Reactant 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 131730213HCID 131730213, compound

Product 1

HCID 131730215HCID 131730215, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

After suspending N-(2-fluoro-4-{[2-({[4-(4-methylpiperazin-1-yl)piperidin-1-yl]carbonyl}amino)pyridin-4-yl]oxy}phenyl)-N′-(4-fluorophenyl)cyclopropane-1,1-dicarboxyamide (31.7 mg) in ethanol (0.317 ml)-water (0.0058 ml), 2.5 M sulfuric acid (0.010 ml) was added at room temperature to form a solution. The solution was stirred overnight at room temperature. The precipitate was collected by filtration and washed with ethanol (0.158 ml, 2 times). It was then dried under aeration at room temperature for 30 minutes, and then dried with warm air at 60° C. for 1 day to give the title compound (26.5 mg) as white powder.

Workup

  1. additionwas added at room temperature
  2. customto form a solution
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with ethanol (0.158 ml, 2 times)
  5. customIt was then dried under aeration at room temperature for 30 minutes
  6. customdried
  7. temperaturewith warm air at 60° C. for 1 day

Sources & evidence

ORD record
ord-c10f8ee8f20c41428e4cada9abd44aad
Source dataset
uspto-grants-2013_02
Patent number
US08377938B2

Reaction notes

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