Hydrochloric Acid → HCID 86691670, compound

HRID 2408900Notes

Reaction equation

HRID 2408900 reaction equation
[ClH:1].[NH2:2][C:3]1[C:4]2[C:5]3[C:6](=[N:18][N:19]([CH2:21][C:22]4[C:27]([Cl:28])=[C:26]([O:29][CH3:30])[C:25]([CH3:31])=[CH:24][N:23]=4)[N:20]=2)[CH:7]=[C:8]([CH2:13][C:14]([NH:16][CH3:17])=[O:15])[C:9]=3[CH2:10][S:11][N:12]=1>CC(C)=O>[ClH:28].[ClH:1].[NH2:2][C:3]1[C:4]2[C:5]3[C:6](=[N:18][N:19]([CH2:21][C:22]4[C:27]([Cl:28])=[C:26]([O:29][CH3:30])[C:25]([CH3:31])=[CH:24][N:23]=4)[N:20]=2)[CH:7]=[C:8]([CH2:13][C:14]([NH:16][CH3:17])=[O:15])[C:9]=3[CH2:10][S:11][N:12]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 666180742-{4-Amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide

Product 1

HCID 86691670HCID 86691670, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

3 M hydrochloric acid (369.6 mL) was added dropwise to an acetone (30 mL) suspension of 2-{4-amino-2-[(3-chloro-4-methoxy-5-methylpyridin-2-yl)methyl]-2,7-dihydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-8-yl}-N-methylacetamide (493.48 mg, 1.11 mmol) at room temperature, while the suspension was stirred. The resulting mixture was further stirred for 12 hours. The obtained crystal was collected by filtration, was then washed with acetone, and was then dried under reduced pressure at 25° C. for 3 hours, so as to obtain the above title compound (531.01 mg, 1.02 mmol). Yield: 92%.

Workup

  1. stirringThe resulting mixture was further stirred for 12 hours
  2. filtrationThe obtained crystal was collected by filtration
  3. washwas then washed with acetone
  4. customwas then dried under reduced pressure at 25° C. for 3 hours

Sources & evidence

ORD record
ord-438a3edd2d424a87a00ab40eff545282
Source dataset
uspto-grants-2014_08
Patent number
US08815880B2

Reaction notes

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