Hydrochloric Acid → Ethyl 3-oxothiomorpholine-2-carboxylate

HRID 483106

反応式

HRID 483106 の反応式
[NH:1]1[CH2:6][CH2:5][S:4][CH2:3][C:2]1=[O:7].C([N-]C(C)C)(C)C.[Li+].Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18].Cl>O1CCCC1>[CH2:20]([O:19][C:17]([CH:3]1[S:4][CH2:5][CH2:6][NH:1][C:2]1=[O:7])=[O:18])[CH3:21]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10928Ethyl chloroformateHCID 884021,4-Tetrahydrothiazine-3-oneHCID 2724682Lithium diisopropylamide

生成物 1

HCID 12858120Ethyl 3-oxothiomorpholine-2-carboxylate収率 80%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of thiomorpholin-3-one (1 equivalent), tetrahydrofuran (5-40 parts), and lithium diisopropylamide (1-2 equivalents) is stirred at -10° to 50° C. for 1 to 3 hours. To this mixture is added ethyl chloroformate (1 to 2 equivalents). After 1 to 3 hours' stirring, the mixture is acidified with hydrochloric acid, concentrated, diluted with ethyl acetate, washed with water, dried, and concentrated to give 3-oxothiomorpholine-2-carboxylic acid ethyl ester in 80 to 90% yield.

後処理

  1. stirringAfter 1 to 3 hours' stirring
  2. concentrationconcentrated
  3. additiondiluted with ethyl acetate
  4. washwashed with water
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-889881e554b3495c8d655e1a7038ac9b
出典データセット
uspto-grants-1986_03
特許番号
US04578378

関連ノート

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