Hydrochloride methanol → HCID 178457211, compound

HRID 2080888Notes

Reaction equation

HRID 2080888 reaction equation
C[N:2]1[CH:6]=[CH:5][N:4]=[C:3]1[CH2:7][N:8]([CH2:34][C:35]1[CH:65]=[CH:64][C:38]([CH2:39][N:40]([CH2:52][C:53]2[N:57](C3CCCCO3)[N:56]=[N:55][N:54]=2)[CH2:41][CH2:42][CH2:43][CH2:44][N:45]([CH2:49][CH2:50][CH3:51])[CH2:46][CH2:47][CH3:48])=[CH:37][CH:36]=1)[CH2:9][C:10]1[N:11]([C:15](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:12]=[CH:13][N:14]=1.Cl.CO>CO>[NH:4]1[CH:5]=[CH:6][N:2]=[C:3]1[CH2:7][N:8]([CH2:34][C:35]1[CH:65]=[CH:64][C:38]([CH2:39][N:40]([CH2:52][C:53]2[NH:57][N:56]=[N:55][N:54]=2)[CH2:41][CH2:42][CH2:43][CH2:44][N:45]([CH2:49][CH2:50][CH3:51])[CH2:46][CH2:47][CH3:48])=[CH:37][CH:36]=1)[CH2:9][C:10]1[N:11]([CH3:15])[CH:12]=[CH:13][N:14]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 67103343HCID 67103343, compound

Product 1

HCID 178457211HCID 178457211, compoundYield 107.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The compound (35.6 mg) obtained in Example 91-4 was dissolved in methanol (0.80 ml) and added with a 10% hydrogen chloride/methanol solution (0.80 ml) and the whole was stirred overnight at room temperature. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was added with ethyl acetate and water, and the aqueous layer was washed with ethylacetate. The aqueous layer was concentrated and evaporated to dryness under reduced pressure, thereby obtaining a hydrochloride (23.9 mg) of the subject compound as a white solid.

Workup

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off under reduced pressure
  3. additionThe residue was added with ethyl acetate and water
  4. washthe aqueous layer was washed with ethylacetate
  5. concentrationThe aqueous layer was concentrated
  6. customevaporated to dryness under reduced pressure

Sources & evidence

ORD record
ord-69c78c1a3bd34c01ba10d59464e34363
Source dataset
uspto-grants-2011_04
Patent number
US07932281B2

Reaction notes

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