Hydrogen chloride-ethyl acetate → HCID 136333927, compound

HRID 1409033Notes

Reaction equation

HRID 1409033 reaction equation
[CH3:1][C:2]1[NH:6][N:5]=[CH:4][C:3]=1[C:7]1[S:15][C:14]2[C:13](=[O:16])[NH:12][C:11]([CH:17](N3CCCC3)[CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[N:10][C:9]=2[CH:8]=1.[ClH:30].C(OCC)(=O)C>CO>[ClH:30].[CH3:1][C:2]1[NH:6][N:5]=[CH:4][C:3]=1[C:7]1[S:15][C:14]2[C:13](=[O:16])[NH:12][C:11](/[CH:17]=[CH:18]/[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[N:10][C:9]=2[CH:8]=1

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 136603356HCID 136603356, compound

Product 1

HCID 136333927HCID 136333927, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of a crude product (5.0 mg) of tert-butyl 3-methyl-4-{4-oxo-2-[(E)-2-phenylethenyl]-3,4-dihydrothieno[3,2-d]pyrimidin-6-yl}-1H-pyrazole-1-carboxylate produced in Example 94, step B, in methanol (1.0 mL) was added 4M hydrochloric acid/ethyl acetate solution (0.50 mL). The reaction system was stirred at room temperature for 30 min, and the mixture was concentrated under reduced pressure. The residue was crystallized from methanol/ethyl acetate to give the title compound (1.7 mg) as a yellow solid.

Workup

  1. concentrationthe mixture was concentrated under reduced pressure
  2. customThe residue was crystallized from methanol/ethyl acetate

Sources & evidence

ORD record
ord-1859fc242c8e40f59394bcb9aa64a028
Source dataset
uspto-grants-2014_12
Patent number
US08921354B2

Reaction notes

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