Hydrochloric Acid → HCID 11397823, compound

HRID 352963Notes

Reaction equation

HRID 352963 reaction equation
Cl.C(OC([N:9]1[C:17]2[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][C:12]=2[CH:11]=[C:10]1[C:25]([N:27]1[CH2:32][CH2:31][N:30]([S:33]([C:36]2[CH:45]=[CH:44][C:43]3[C:38](=[CH:39][CH:40]=[C:41]([Cl:46])[CH:42]=3)[CH:37]=2)(=[O:35])=[O:34])[CH2:29][CH2:28]1)=[O:26])=O)(C)(C)C>C(O)C>[ClH:46].[Cl:46][C:41]1[CH:42]=[C:43]2[C:38](=[CH:39][CH:40]=1)[CH:37]=[C:36]([S:33]([N:30]1[CH2:31][CH2:32][N:27]([C:25]([C:10]3[NH:9][C:17]4[CH2:16][CH2:15][NH:14][CH2:13][C:12]=4[CH:11]=3)=[O:26])[CH2:28][CH2:29]1)(=[O:35])=[O:34])[CH:45]=[CH:44]2

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 11227605HCID 11227605, compound

Product 1

HCID 11397823HCID 11397823, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A saturated solution of hydrochloride in ethanol (25 ml) was added to 1,5-bis(t-butoxycarbonyl)-2-[[4-[(6-chloronaphthalen-2-yl)sulfonyl]piperazin-1-yl]carbonyl]-4,5,6,7-tetrahydro-1H-pyrrolo[3,2-c]pyridine (300 mg) at room temperature, followed by stirring for 1 hour. The reaction mixture was concentrated and water was added to the concentrate. The resulting mixture was concentrated under reduced pressure. To the residue, a saturated solution of hydrochloride in methanol (25 ml) was added at room temperature, followed by stirring for 1 hour. After concentration of the reaction mixture, water was added and the resulting mixture was concentrated under reduced pressure, whereby the title compound (200 mg) was obtained as a white solid.

Workup

  1. concentrationThe reaction mixture was concentrated
  2. additionwater was added to the concentrate
  3. concentrationThe resulting mixture was concentrated under reduced pressure
  4. additionTo the residue, a saturated solution of hydrochloride in methanol (25 ml) was added at room temperature
  5. stirringby stirring for 1 hour
  6. additionAfter concentration of the reaction mixture, water was added
  7. concentrationthe resulting mixture was concentrated under reduced pressure, whereby the title compound (200 mg)
  8. customwas obtained as a white solid

Sources & evidence

ORD record
ord-8570038abb754dd2806eb77eb3d6acf0
Source dataset
uspto-grants-2004_06
Patent number
US06747023B1

Reaction notes

Loading…