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Potassium Hydroxide → HCID 86639224、化合物

HRID 1511615
ノート
印刷プレビュー

反応式

HRID 1511615 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][N:7]([CH:15]=[O:16])[CH2:8][CH2:9][C:10]([O:12]CC)=[O:11].[OH-].[K+]>C(O)C>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][N:7]([CH:15]=[O:16])[CH2:8][CH2:9][C:10]([OH:12])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 86639223HCID 86639223、化合物

生成物 1

HCID 86639224HCID 86639224、化合物収率 100.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl 3-[(thiophen-2-ylmethyl) (formyl)amino]-propionate (15.6 g) prepared in the step 2 was added to a solution of 5.4 g of potassium hydroxide in 100 mL of ethanol and stirred at room temperature for 2 hours. The solvent was evaporated from the reaction solution in vacuo, 50 mL of water was added to the residue and the mixture was subjected to extraction with diethyl ether. The resulting aqueous solution was slowly neutralized with a 1N aqueous solution of hydrochloric acid with stirring to adjust to pH 3 followed by extracting with diethyl ether. The organic layer was separated, washed with water and a saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom in vacuo to give 13.8 g of the objective compound as light yellow liquid.

後処理

  1. customThe solvent was evaporated from the reaction solution in vacuo, 50 mL of water
  2. additionwas added to the residue
  3. extractionthe mixture was subjected to extraction with diethyl ether
  4. stirringwith stirring
  5. extractionby extracting with diethyl ether
  6. customThe organic layer was separated
  7. washwashed with water
  8. dry with materiala saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate
  9. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-b931a19df6474b24afef1e2eb6b73e3e
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217031B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート