Hydroxyamine hydrochloride → Ethyl 2-oximinooxamate

HRID 236987

反応式

HRID 236987 の反応式
[Na].Cl.[NH2:3][OH:4].[CH3:5][CH2:6][O:7][C:8]([C:10]([NH2:12])=S)=[O:9]>C(O)C>[CH3:5][CH2:6][O:7][C:8](/[C:10](/[NH2:12])=[N:3]/[OH:4])=[O:9]

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 2733398Ethyl thiooxamateHCID 5360545Sodium

生成物 1

HCID 9614369Ethyl 2-oximinooxamate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution of 8.98 gm. (0.39 mole) of sodium in 180 ml. of anhydrous ethanol is added to a solution of 26.8 gm. (0.386 mole) of hydroxylamine hydrochloride in 270 ml. of hot ethanol. The precipitate is removed by filtration. To the stirred filtrate is added 34.2 gm. (0.26 mole) of ethyl 2-thiooxamate. The yellow solution is allowed to stand overnight. The solution is evaporated to dryness in vacuo and the residue recrystallized from diethyl ether. There is obtained 21.2 g. (68%) of a yellow solid melting at 99°-101° C.

後処理

  1. customThe precipitate is removed by filtration
  2. additionTo the stirred filtrate is added 34.2 gm
  3. customThe solution is evaporated to dryness in vacuo
  4. customthe residue recrystallized from diethyl ether
  5. customThere is obtained 21.2 g

出典と根拠

ORDレコード
ord-2038fc3009464cafb1a1921d9b62ec37
出典データセット
uspto-grants-1979_06
特許番号
US04159336

関連ノート

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