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Potassium Hydroxide → [3-(5-Chloro-2-thienyl)-4-(2-methoxyethyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]acetic acid

HRID 709149
ノート
印刷プレビュー

反応式

HRID 709149 の反応式
[Cl:1][C:2]1[S:6][C:5]([C:7]2[N:11]([CH2:12][CH2:13][O:14][CH3:15])[C:10](=[O:16])[N:9]([CH2:17][C:18]([O:20]CC)=[O:19])[N:8]=2)=[CH:4][CH:3]=1.[OH-].[K+]>CO>[Cl:1][C:2]1[S:6][C:5]([C:7]2[N:11]([CH2:12][CH2:13][O:14][CH3:15])[C:10](=[O:16])[N:9]([CH2:17][C:18]([OH:20])=[O:19])[N:8]=2)=[CH:4][CH:3]=1
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 59536780Ethyl [3-(5-chloro-2-thienyl)-4-(2-methoxyethyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]acetate

生成物 1

HCID 59536891[3-(5-Chloro-2-thienyl)-4-(2-methoxyethyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]acetic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3.2 g (9.25 mmol) of the compound of Example 51A were dissolved in 28 ml of methanol. 2.82 ml of a 20% strength aqueous potassium hydroxide solution were then added. The mixture was stirred at RT for 2 h. On a rotary evaporator, the proportion of methanol was reduced by half. The mixture was then diluted with water and extracted once with 15 ml of ethyl acetate. The aqueous phase was acidified with 920 μl of concentrated hydrochloric acid and extracted twice with in each case 15 ml of ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and freed from the solvent on a rotary evaporator. Drying the residue under high vacuum gave 2.34 g (80% of theory) of the title compound.

後処理

  1. customOn a rotary evaporator
  2. additionThe mixture was then diluted with water
  3. extractionextracted once with 15 ml of ethyl acetate
  4. extractionextracted twice with in each case 15 ml of ethyl acetate
  5. dry with materialThe combined organic phases were dried over sodium sulphate
  6. filtrationfiltered
  7. customfreed from the solvent on a rotary evaporator
  8. customDrying the residue under high vacuum

出典と根拠

ORDレコード
ord-ae7bc03dd2fd4c34bbf02d9dc40a8b45
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09180120B2

反応ノート

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