Hydrochloric Acid → HCID 44476317, compound

HRID 1693274Notes

Reaction equation

HRID 1693274 reaction equation
[C:1]([CH:3]1[CH2:13][C:12]2[C:14]3[C:9]([N:10]([CH2:15][C:16]4[C:21]([CH3:22])=[C:20]([O:23][CH3:24])[C:19]([CH3:25])=[CH:18][N:17]=4)[N:11]=2)=[N:8][C:7]([N:26](C(OC(C)(C)C)=O)C(OC(C)(C)C)=O)=[N:6][C:5]=3[S:4]1)#[N:2].C[O:42]C1C(C)=CN=C(CN2C3C4C(CC(C)SC=4N=C(N)N=3)=N2)C=1C.Cl.C(=O)(O)[O-].[Na+]>O>[NH2:26][C:7]1[N:8]=[C:9]2[C:14]3[C:12]([CH2:13][CH:3]([C:1]([NH2:2])=[O:42])[S:4][C:5]=3[N:6]=1)=[N:11][N:10]2[CH2:15][C:16]1[C:21]([CH3:22])=[C:20]([O:23][CH3:24])[C:19]([CH3:25])=[CH:18][N:17]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 24811286HCID 24811286, compoundHCID 44476495HCID 44476495, compound

Product 1

HCID 44476317HCID 44476317, compoundYield 91%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture composed of di-tert-butyl {7-cyano-2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-7,8-dihydro-2H-6-thia-1,2,3,5-tetraazaacenaphthylen-4-yl}imidodicarbonate of Step 4) of Example 3 (30 mg) and concentrated hydrochloric acid (1 mL) was stirred at room temperature for 1.5 hours. The reaction mixture was diluted with water and neutralized with a saturated sodium bicarbonate solution. The precipitate was collected by filtration and sequentially washed with a saturated sodium bicarbonate solution and water. Then, the resulting solid was dried to obtain the title compound (18.5 mg, 91%).

Workup

  1. filtrationThe precipitate was collected by filtration
  2. washsequentially washed with a saturated sodium bicarbonate solution and water
  3. customThen, the resulting solid was dried

Sources & evidence

ORD record
ord-e66750d68f5a48f5bc04f744a794fad5
Source dataset
uspto-grants-2012_04
Patent number
US08158638B2

Reaction notes

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