Reaktion #54461

ord-e699c697c18f4bd396844235484c158f

Reaktionsgleichung

[Li+].[NH2-]
lithium amide
COC(=O)CS(=O)(=O)C(C)(C)C
methyl t-butylsulphonyl-acetate
CC1(C)CC(O)CC(C)(C)N1
4-hydroxy-2,2,6,6-tetramethylpiperidine
CC1(C)CC(OC(=O)CS(=O)(=O)C(C)(C)C)CC(C)(C)N1
2,2,6,6-tetramethyl-4-piperidinyl t-butyl-sulphonyl-acetate

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is warmed to 130°
  2. 2
    SonstigeThe xylene is removed in vacuo
  3. 3
    workup.DISTILLATIONthe residue is distilled

Vorschrift

38.8 g (0.2 mol) of methyl t-butylsulphonyl-acetate, prepared according to the method of von Leusen and Strating, Rec. Trav, Chim. 84, 140 (1965), and 31.4 g (0.2 mol) of 4-hydroxy-2,2,6,6-tetramethylpiperidine are dissolved in 50 ml of xylene. The mixture is warmed to 130°, 0.2 g of lithium amide in 50 ml of xylene is added and the mixture is stirred for 12 hours at 130°-140°. The xylene is removed in vacuo and the residue is distilled to give 2,2,6,6-tetramethyl-4-piperidinyl t-butyl-sulphonyl-acetate; yield: 33.7 grams, boiling point 153°-154°/10-3 mm Hg.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04148784uspto-grants-1979_04