Ethanolamine → N-(2-hydroxyethyl)-p-(2-thenoyl)hydratropamide

HRID 461746ノート

反応式

HRID 461746 の反応式
[NH2:1][CH2:2][CH2:3][OH:4].[C:5]1([C:10]([C:12]2[CH:22]=[CH:21][C:15]([CH:16]([CH3:20])[C:17](Cl)=[O:18])=[CH:14][CH:13]=2)=[O:11])[S:9][CH:8]=[CH:7][CH:6]=1>C(Cl)(Cl)Cl>[OH:4][CH2:3][CH2:2][NH:1][C:17](=[O:18])[CH:16]([C:15]1[CH:14]=[CH:13][C:12]([C:10](=[O:11])[C:5]2[S:9][CH:8]=[CH:7][CH:6]=2)=[CH:22][CH:21]=1)[CH3:20]

参加物

4

反応物 2

HCID 700EthanolamineHCID 11747905p-(2-Thenoyl)hydratropoyl chloride

生成物 1

HCID 12232965N-(2-hydroxyethyl)-p-(2-thenoyl)hydratropamide

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a stirred solution of 2.44 parts of 2-aminoethanol in 15 parts of chloroform is added dropwise a solution of 5.6 parts of p-(2-thenoyl)hydratropoyl chloride in 15 parts of chloroform at room temperature (highly exothermic reaction). Upon completion, the whole is stirred and refluxed for 1 hour. The reaction mixture is cooled and washed with a 1N hydrochloric acid solution. The organic layer is separated, washed twice with water, dried, filtered and evaporated. The oily residue solidifies on triturating in petroleumether. The solid product is filtered off and crystallized from boiling ether, yielding N-(2-hydroxyethyl)-p-(2-thenoyl)hydratropamide; m.p. 87.1° C.

後処理

  1. customhighly exothermic reaction)
  2. temperaturerefluxed for 1 hour
  3. temperatureThe reaction mixture is cooled
  4. washwashed with a 1N hydrochloric acid solution
  5. customThe organic layer is separated
  6. washwashed twice with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customon triturating in petroleumether
  11. filtrationThe solid product is filtered off
  12. customcrystallized

出典と根拠

ORDレコード
ord-a9e41c60a2a04d6d817f6887c40a5bea
出典データセット
uspto-grants-1977_12
特許番号
US04064132

反応ノート

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