Triethylamine → HCID 13120688, compound
Reaction equation
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]1[N:11]([CH2:12][CH2:13][OH:14])[CH2:10][CH2:9][NH:8][C:7]1=[O:15].C(N(CC)CC)C.[Cl:23][C:24]1[CH:34]=[CH:33][C:27]([O:28][CH2:29][C:30](Cl)=[O:31])=[CH:26][CH:25]=1>C(Cl)(Cl)Cl>[ClH:23].[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]1[N:11]([CH2:12][CH2:13][O:14][C:30]([CH2:29][O:28][C:27]2[CH:33]=[CH:34][C:24]([Cl:23])=[CH:25][CH:26]=2)=[O:31])[CH2:10][CH2:9][NH:8][C:7]1=[O:15]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
18.1 g (0.08 mol) of 3-(2-thienyl)-4-hydroxyethylpiperazin-2-one, prepared in accordance with Example 27, are dissolved in 160 ml of chloroform and acylated with 10.1 g (0.1 mol) of triethylamine and 20.5 g (0.1 mol) of 4-chlorophenoxyacetyl chloride. The mixture is stirred for a further 4 hours at room temperature and evaporated, and the residue is extracted by shaking with ethyl acetate. The ethyl acetate extract is dried with sodium sulphate, and the compound is precipitated as the hydrochloride by adding hydrochloric acid in ether.
Workup
- customevaporated
- extractionthe residue is extracted
- stirringby shaking with ethyl acetate
- extractionThe ethyl acetate extract
- dry with materialis dried with sodium sulphate
- customthe compound is precipitated as the hydrochloride
- additionby adding hydrochloric acid in ether
Sources & evidence
- ORD record
- ord-d5b7d6363f0d4a22b7c63cbeb105e167
- Source dataset
- uspto-grants-1986_07
- Patent number
- US04598079
Reaction notes
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