Hydrochloric Acid → HCID 71224201, compound

HRID 2402956Notes

Reaction equation

HRID 2402956 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[N:9]1[C:14](=[O:15])[C:13]2[CH:16]=[N:17][C:18]([NH:20][C:21]3[CH:26]=[CH:25][C:24]([N:27]4[CH2:32][CH2:31][N:30]([CH3:33])[CH2:29][CH2:28]4)=[CH:23][CH:22]=3)=[N:19][C:12]=2[C:11]([C:34]2[CH:39]=[CH:38][N:37]=[C:36]([C:40]([O:42]C)=[O:41])[CH:35]=2)=[N:10]1.O.[OH-].[Li+].CO.Cl>C1COCC1.O>[Cl:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]=1[N:9]1[C:14](=[O:15])[C:13]2[CH:16]=[N:17][C:18]([NH:20][C:21]3[CH:22]=[CH:23][C:24]([N:27]4[CH2:32][CH2:31][N:30]([CH3:33])[CH2:29][CH2:28]4)=[CH:25][CH:26]=3)=[N:19][C:12]=2[C:11]([C:34]2[CH:39]=[CH:38][N:37]=[C:36]([C:40]([OH:42])=[O:41])[CH:35]=2)=[N:10]1

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 71224181HCID 71224181, compound

Product 1

HCID 71224201HCID 71224201, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

To a solution of Example 222 (0.36 g, 0.583 mmol) in THF (8 mL) was added lithium hydroxide monohydrate (0.049 g, 1.166 mmol) in water (8 mL). Methanol was added until a transparent solution formed (8 mL). This mixture was stirred at room temperature for 2 hours and acidified to pH 5 with 2N aqueous HCl solution. The mixture was concentrated and the formed solid was collected by filtration, washed with water and dried to give the title compound. MS (DCI/NH3) m/z 604 (M+H)+.

Workup

  1. customformed (8 mL)
  2. concentrationThe mixture was concentrated
  3. filtrationthe formed solid was collected by filtration
  4. washwashed with water
  5. customdried

Sources & evidence

ORD record
ord-5d2027cb7e9d4d58b50a7d5a671ef13c
Source dataset
uspto-grants-2014_08
Patent number
US08796289B2

Reaction notes

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