Triethylamine → Acesulfame

HRID 1732098

反応式

HRID 1732098 の反応式
C(N(CC)CC)C.[C:8]([NH2:14])(=[O:13])[CH2:9][C:10]([CH3:12])=[O:11].Cl[S:16](F)(=[O:18])=[O:17]>>[CH3:12][C:10]1[O:11][S:16](=[O:18])(=[O:17])[NH:14][C:8](=[O:13])[CH:9]=1

参加物

4

反応物 3

HCID 8471TriethylamineHCID 26159Sulfuryl chloride fluorideHCID 80077Acetoacetamide

生成物 1

HCID 36573Acesulfame収率 46%

実験手順

A mixture, with a total volume of 50 ml, of 40.4 g (0.4 mol) of triethylamine and liquid SO2 was added dropwise, at -10° C., to a solution of 20.2 g (0.2 mol) of acetoacetamide and 23.7 g (0.2 mol) of chlorosulfonyl fluoride in 70 ml of liquid SO2. The mixture was stirred for 2 hours and the liquid SO2 was then distilled off, a vacuum being applied at the end. The residue was added dropwise to 400 ml of aqueous NaOH, acidified with concentrated hydrochloric acid, with ice-cooling, and extracted with ethyl acetate. After treatment of the ethyl acetate phase with animal charcoal and Na2SO4, the extract was evaporated in vacuo. 15 g (approx. 20% of theory) of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide were obtained.

後処理

  1. distillationthe liquid SO2 was then distilled off
  2. additionThe residue was added dropwise to 400 ml of aqueous NaOH
  3. temperaturecooling
  4. extractionextracted with ethyl acetate
  5. customAfter treatment of the ethyl acetate phase with animal charcoal and Na2SO4, the extract was evaporated in vacuo

出典と根拠

ORDレコード
ord-35384e460b1e4317b7aa20fbd63a113b
出典データセット
uspto-grants-1986_11
特許番号
US04625024

関連ノート

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