Hydrochloric Acid → HCID 19374875, compound

HRID 128690Notes

Reaction equation

HRID 128690 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

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

  1. temperaturecool
  2. extractionExtract with methylene chloride
  3. extractionAlkanilise the aqueous phase with sodium carbonate and extract with methylene chloride
  4. customDry the organic phase
  5. customevaporate under vacuum
  6. customPurify the residue by chromatography on a silica column
  7. 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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