Hydrochloric Acid → HCID 19374875, compound
Reaction equation
Cl.C([NH:10][C:11](=[S:25])[N:12]([CH:16]([C:18]1[CH:23]=[CH:22][N:21]=[CH:20][C:19]=1[Cl:24])[CH3:17])[CH2:13][CH2:14][CH3:15])(=O)C1C=CC=CC=1>O>[Cl:24][C:19]1[CH:20]=[N:21][CH:22]=[CH:23][C:18]=1[CH:16]([N:12]([CH2:13][CH2:14][CH3:15])[C:11]([NH2:10])=[S:25])[CH3:17]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Add 6 ml of 32% hydrochloric acid to 1.18 g of the compound obtained in Step A. Bring the reaction medium to 80° C. for one hour, then cool and add water. Extract with methylene chloride and discard the organic phase. Alkanilise the aqueous phase with sodium carbonate and extract with methylene chloride. Dry the organic phase and evaporate under vacuum. Purify the residue by chromatography on a silica column, using a mixture of methylene chloride and methanol (98:2 V/V) as eluent.
Workup
- temperaturecool
- extractionExtract with methylene chloride
- extractionAlkanilise the aqueous phase with sodium carbonate and extract with methylene chloride
- customDry the organic phase
- customevaporate under vacuum
- customPurify the residue by chromatography on a silica column
- additiona mixture of methylene chloride and methanol (98:2 V/V) as eluent
Sources & evidence
- ORD record
- ord-0a6fbf346934482d880efff9a5832b05
- Source dataset
- uspto-grants-1995_11
- Patent number
- US05464847
Reaction notes
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