Hydrochloric Acid → HCID 15308001, compound

HRID 1938324Notes

Reaction equation

HRID 1938324 reaction equation
[Cl:1][C:2]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:3]=1[C:4]([NH:6][C:7]1[CH:34]=[CH:33][C:10]([C:11]([N:13]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=3[C:17]3=[N:24][N:25]([CH2:27][C:28]([O:30]CC)=[O:29])[CH:26]=[C:16]3[CH2:15][CH2:14]2)=[O:12])=[CH:9][CH:8]=1)=[O:5].O1CCCC1.[OH-].[Na+].Cl>C(O)C>[Cl:1][C:2]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:3]=1[C:4]([NH:6][C:7]1[CH:34]=[CH:33][C:10]([C:11]([N:13]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=3[C:17]3=[N:24][N:25]([CH2:27][C:28]([OH:30])=[O:29])[CH:26]=[C:16]3[CH2:15][CH2:14]2)=[O:12])=[CH:9][CH:8]=1)=[O:5]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 18940516Ethyl 6-[4-[(2,4-dichlorobenzoyl)amino]benzoyl]-5,6-dihydropyrazolo[4,3-d][1]benzazepine-2(4H)-acetate

Product 1

HCID 15308001HCID 15308001, compoundYield 0.1%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a stirred slurry of 0.477 g of 6-[4-[(2,4-dichlorobenzoyl)amino]benzoyl]-5,6-dihydropyrazolo-[4,3-d][1]benzazepine-2(4H)-acetic acid, ethyl ester in 15 ml of ethyl alcohol is added 5 ml of tetrahydrofuran followed by 1.30 ml of 1M NaOH. The reaction mixture is stirred at room temperature for 6 hours followed by the addition of 0.750 ml of 2M HCl. The acidic reaction mixture is evaporated in vacuo, triturated with CHCl3, combined, treated with activated carbon, filtered through MgSO4 and evaporated in vacuo to give 0.380 mg of the desired product as a clear foam.

Workup

  1. customThe acidic reaction mixture is evaporated in vacuo
  2. customtriturated with CHCl3
  3. additiontreated with activated carbon
  4. filtrationfiltered through MgSO4
  5. customevaporated in vacuo

Sources & evidence

ORD record
ord-ed2b72a63af44a3ba759e0da578376c0
Source dataset
uspto-grants-1997_12
Patent number
US05693635

Reaction notes

Loading…