HCID 131720471, compound → HCID 131720473, compound

HRID 862570Notes

Reaction equation

HRID 862570 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]2[CH2:16][CH2:15][C@@H:14]([CH2:17][C:18](=[O:38])[NH:19][C:20]3[CH:25]=[CH:24][C:23]([CH2:26][NH:27]C(OC(C)(C)C)=O)=[CH:22][C:21]=3[C:35]([OH:37])=[O:36])[N:6]3[C:7](=[O:13])[C:8](=[O:12])[NH:9][C:10]([CH:11]=1)=[C:5]23>Cl.O1CCOCC1.C(OCC)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]2[CH2:16][CH2:15][C@@H:14]([CH2:17][C:18](=[O:38])[NH:19][C:20]3[CH:25]=[CH:24][C:23]([CH2:26][NH2:27])=[CH:22][C:21]=3[C:35]([OH:37])=[O:36])[N:6]3[C:7](=[O:13])[C:8](=[O:12])[NH:9][C:10]([CH:11]=1)=[C:5]23

Participants

5

Reactant 1

HCID 131720471HCID 131720471, compound

Product 1

HCID 131720473HCID 131720473, compoundYield 184.4%

Reagents, catalysts & solvents 3

HCID 313Hydrochloric AcidSolventHCID 3283Diethyl EtherSolventHCID 312751,4-DioxaneSolvent

Procedure

A suspension of (S)-9-chloro-5-(p-tert-butoxycarbonylaminomethyl-o-carboxyphenylcarbamoylmethyl)-6,7-dihydro-1H, 5H-pyrido[1,2,3-de]-quinoxaline-2,3-dione (430 mg) in 2N hydrogen chloride in 1,4-dioxane (14 mL) was stirred overnight at room temperature and diluted with diethyl ether. The precipitates were collected by filtration and recrystallized from water to give 350 mg of the title compound.

Workup

  1. filtrationThe precipitates were collected by filtration
  2. customrecrystallized from water

Sources & evidence

ORD record
ord-369a6e40c17443e7bef16f4c0c911a76
Source dataset
uspto-grants-1998_02
Patent number
US05719152

Reaction notes

Loading…