Hydrochloric Acid → HCID 13054054, compound
Reaction equation
Cl.[Cl:2][C:3]1[CH:20]=[CH:19][CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH2:11][CH2:10][C:9](=[O:12])[CH:8]([CH2:13][C:14]([OH:16])=[O:15])[CH2:7]1.Cl.[CH3:22]O>>[CH3:22][O:15][C:14](=[O:16])[CH2:13][CH:8]1[C:9](=[O:12])[CH2:10][CH2:11][N:6]([CH2:5][C:4]2[CH:17]=[CH:18][CH:19]=[CH:20][C:3]=2[Cl:2])[CH2:7]1Participants
4
Procedure
A solution of 30 g. of this hydrochloride in 300 cc. methanol saturated with gaseous hydrogen chloride is stirred at ambient temperature for 3 hours. The reaction mixture is then evaporated in a vacuum at a temperature below 50° C. and the residue is poured into water, rendered basic by the addition of sodium bicarbonate and extracted with methylene chloride. The organic extracts are washed with water, dried with anhydrous sodium sulphate and evaporated to dryness. The yellow resin obtained is used, without further purification, for the following stage.
Workup
- customThe reaction mixture is then evaporated in a vacuum at a temperature below 50° C.
- additionthe residue is poured into water
- additionrendered basic by the addition of sodium bicarbonate
- extractionextracted with methylene chloride
- washThe organic extracts are washed with water
- dry with materialdried with anhydrous sodium sulphate
- customevaporated to dryness
- customThe yellow resin obtained
- customis used, without further purification, for the following stage
Sources & evidence
- ORD record
- ord-7346274ceb514958956162d1013d0f21
- Source dataset
- uspto-grants-1984_01
- Patent number
- US04424356
Reaction notes
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