Hydrochloric Acid → HCID 86752470, compound

HRID 1600075Notes

Reaction equation

HRID 1600075 reaction equation
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][NH:10][C:11](=[O:31])[C@@H:12]2[CH2:16][CH2:15][CH2:14][N:13]2[C:17](=[O:30])[CH2:18][C@H:19]2[CH2:24][CH2:23][CH2:22][CH2:21][CH:20]2[NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[CH:5][CH:4]=1)#[N:2].[ClH:32].C(=O)([O-])[O-].[NH4+:37].[NH4+]>C(O)C>[Cl-:32].[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH2:9][NH:10][C:11](=[O:31])[C@@H:12]2[CH2:16][CH2:15][CH2:14][N:13]2[C:17](=[O:30])[CH2:18][C@H:19]2[CH2:24][CH2:23][CH2:22][CH2:21][CH:20]2[NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[CH:7][CH:8]=1)(=[NH:37])[NH2:2]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 517111Ammonium CarbonateHCID 86752469HCID 86752469, compound

Product 1

HCID 86752470HCID 86752470, compoundYield 73%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of the compound (18.6 g, 42 mmol) obtained in the item (d) inchloroform (100 ml), a 37% hydrochloride in ethanol (100 ml) is added at 0° C. The mixture is allowed to stand at 0° C. for 48 hours and then the solvent is evaporated. The resulting residue is dissolved in methanol (100 ml) and ammonium carbonate (16 g, 166 mmol) is added at 0° C. After stirring for 6 hours, the solvent is evaporated and theresulting residue is purified with silica gel chromatography (chloroform-methanol) to give 5.2 g of the titled compound (73%).

Workup

  1. customthe solvent is evaporated
  2. dissolutionThe resulting residue is dissolved in methanol (100 ml)
  3. customthe solvent is evaporated
  4. customresidue is purified with silica gel chromatography (chloroform-methanol)

Sources & evidence

ORD record
ord-1f0f8c8187cb45ea8120d9a7439fd183
Source dataset
uspto-grants-1998_04
Patent number
US05744487

Reaction notes

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