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Triethylamine → HCID 13120688, compound

HRID 745236
Notes
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Reaction equation

HRID 745236 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]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 77771p-Chlorophenoxyacetyl chlorideHCID 30700214-(2-Hydroxyethyl)-3-(thiophen-2-yl)-3,4,5,6-tetrahydropyrazin-2-ol

Product 1

HCID 13120688HCID 13120688, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

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

  1. customevaporated
  2. extractionthe residue is extracted
  3. stirringby shaking with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. dry with materialis dried with sodium sulphate
  6. customthe compound is precipitated as the hydrochloride
  7. additionby adding hydrochloric acid in ether

Sources & evidence

ORD record
ord-d5b7d6363f0d4a22b7c63cbeb105e167
Source dataset
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04598079

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes