Reaktion #1064149

ord-b6b1205ffcf04966b6c5f6167c66c676

Reaktionsgleichung

NCCS
2-aminoethanethiol
CCN(CC)CC
triethylamine
CCOC(=O)C(Br)CBr
ethyl 2,3-dibromopropionate
Cc1ccccc1.ClC(Cl)Cl
chloroform toluene
CCOC(=O)C1CSCCN1
title product
CCOC(=O)C1CSCCN1
Ethyl 3-thiomorpholinecarboxylate

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationfiltered
  2. 2
    Einengenconcentrated in vacuo
  3. 3
    Sonstigeto obtain an orange liquid
  4. 4
    workup.DISTILLATIONdistilled

Vorschrift

A warm solution of 2-aminoethanethiol (10.0 g, 0.130 mol) and triethylamine (36 mL, 0.260 mol) in chloroform is added over 5 minutes to a solution of ethyl 2,3-dibromopropionate (33.9 g, 0.130 mol) in a chloroform/toluene (1:1.6) solution. The reaction mixture is stirred at room temperature for 2.5 hours, filtered and concentrated in vacuo to obtain an orange liquid. The liquid is vacuum distilled to give the title product as a colorless liquid, bp 121°-124° C. at 3 mm Hg.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05612481uspto-grants-1997_03