Hydrogen chloride-ethyl acetate → HCID 131730986, compound

HRID 2035519Notes

Reaction equation

HRID 2035519 reaction equation
[CH2:1]([NH:8][C:9]1[CH:14]=[C:13]([NH:15][C:16]2[CH:21]=[CH:20][C:19]([NH:22][C:23]([CH:25]3[CH2:30][CH2:29][CH2:28][N:27](C(OC(C)(C)C)=O)[CH2:26]3)=[O:24])=[CH:18][CH:17]=2)[N:12]=[CH:11][C:10]=1[CH2:38][C:39]([NH2:41])=[O:40])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(NC1C=C(NC2C=CC(NC(C3CN(C(OC(C)(C)C)=O)C=CC=3)=O)=CC=2)N=CC=1CC(N)=O)C1C=CC=CC=1.[ClH:83].C(OCC)(=O)C>CO>[ClH:83].[CH2:1]([NH:8][C:9]1[CH:14]=[C:13]([NH:15][C:16]2[CH:17]=[CH:18][C:19]([NH:22][C:23]([CH:25]3[CH2:30][CH2:29][CH2:28][NH:27][CH2:26]3)=[O:24])=[CH:20][CH:21]=2)[N:12]=[CH:11][C:10]=1[CH2:38][C:39]([NH2:41])=[O:40])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

5

Reactant 3

HCID 21866389Hydrogen chloride-ethyl acetateHCID 131730985HCID 131730985, compoundHCID 131730988HCID 131730988, compound

Product 1

HCID 131730986HCID 131730986, compoundYield 91%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

25.9 mg of 4-(benzylamino)-6-[(4-{[1-(tert-butoxycarbonyl)piperidin-3-ylcarbonyl]amino}phenyl)amino]pyridine-3-carboxyamide (the compound of Example 308) was dissolved in 1 mL of methanol, to which 1 mL of 4 mol/L hydrochloric acid-ethyl acetate was added, and stirred at room temperature for 30 minutes. The solvent was evaporated, ether was added to the residue, the deposited crystals were filtered to obtain 20.7 mg (91%) of the title compound as a light brown crystalline powder.

Workup

  1. additionwas added
  2. customThe solvent was evaporated
  3. additionether was added to the residue
  4. filtrationthe deposited crystals were filtered

Sources & evidence

ORD record
ord-5a11a88795814daaaaa2887091a9bc91
Source dataset
uspto-grants-2013_11
Patent number
US08575153B2

Reaction notes

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