Reaktion #50498

ord-8f1254ff4e444251aa6e300203244d87

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    SonstigeSubsequently, the volatile materials were removed at a bath temperature of less than 50° C. under 5 mmHg
  3. 3
    SonstigeThe inorganic materials were removed from the residue by filtration

Vorschrift

Trimethylenediamine (37 g) was dissolved in 120 ml of acetonitrile, and a solution of 14.8 g of 5-chloromethyl-2-methylthiazole in 30 ml of acetonitrile was added dropwise at 10° to 15° C. After the addition, the mixture was stirred at 30° to 40° C. for a while, and then 8 g of a 50% aqueous solution of sodium hydroxide was added. Subsequently, the volatile materials were removed at a bath temperature of less than 50° C. under 5 mmHg. The inorganic materials were removed from the residue by filtration to give 16.7 g of N-(2-methyl-5-thiazolylmethyl)trimethylenediamine (purity about 90%) as a colorless oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05428032uspto-grants-1995_06