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Potassium Hydroxide → {2-[(Methylcarbamoyl)amino]-1,3-thiazol-4-yl}acetic acid

HRID 127114
ノート
印刷プレビュー

反応式

HRID 127114 の反応式
[CH3:1][NH:2][C:3](=[O:16])[NH:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][C:11]([O:13]CC)=[O:12])[N:9]=1.[OH-].[K+]>CO.O>[CH3:1][NH:2][C:3](=[O:16])[NH:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][C:11]([OH:13])=[O:12])[N:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 20288637Ethyl {2-[(methylcarbamoyl)amino]-1,3-thiazol-4-yl}acetate

生成物 1

HCID 20288645{2-[(Methylcarbamoyl)amino]-1,3-thiazol-4-yl}acetic acid収率 85.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of ethyl 2-(3-methylureido)thiazol-4-ylacetate (12.8 g.) in a mixture of methanol (240 ml.) and water (240 ml.) was dropwise added 1 N potassium hydroxide aqueous solution (52.7 ml.) with stirring at room temperature, and the solution was stirred for overnight at the same temperature, and then methanol was distilled off therefrom under reduced pressure. The remaining aqueous layer was washed with ethyl acetate, and then 1 N hydrochloric acid (52.7 ml.) was added thereto under ice-cooling. The precipitated crystals were collected by filtration, washed with water and then dried to give colorless crystals of 2-(3-methylureido)thiazol-4-ylacetic acid (9.7 g.), mp 190° C. (dec.).

後処理

  1. stirringthe solution was stirred for overnight at the same temperature
  2. distillationmethanol was distilled off
  3. washThe remaining aqueous layer was washed with ethyl acetate
  4. addition1 N hydrochloric acid (52.7 ml.) was added
  5. temperatureunder ice-cooling
  6. filtrationThe precipitated crystals were collected by filtration
  7. washwashed with water
  8. customdried

出典と根拠

ORDレコード
ord-7a0f1198a66b4233988745ff78fc7b87
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04254260

反応ノート

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