反応 #1569

ord-0ea27041f7c3480cb095d9b064085a09

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過filtered
  2. 2
    濃縮concentrated in vacuo
  3. 3
    その他to obtain an orange liquid
  4. 4
    workup.DISTILLATIONdistilled

実験手順

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-di-bromopropionate (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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726126uspto-grants-1998_03