Acetic Anhydride → 5-Formamido-1-(2-hydroxyethyl)pyrazole

HRID 248334

反応式

HRID 248334 の反応式
[C:1](OC(=O)C)(=[O:3])C.[OH:8][CH2:9][CH2:10][N:11]1[C:15]([NH2:16])=[CH:14][CH:13]=[N:12]1.C(=O)([O-])[O-].[K+].[K+]>C(O)=O>[OH:8][CH2:9][CH2:10][N:11]1[C:15]([NH:16][CH:1]=[O:3])=[CH:14][CH:13]=[N:12]1

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 3202812-(5-amino-1H-pyrazol-1-yl)ethan-1-ol

生成物 1

HCID 150777375-Formamido-1-(2-hydroxyethyl)pyrazole

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

A mixture of acetic anhydride (44.5 ml) and formic acid (22.3 ml) was stirred at ambient temperature for an hour. To this mixture was added 1-(2-hydroxyethyl)-5-aminopyrazole (30 g) at 0°-10° C., and the mixture was stirred under ice-cooling for 30 minutes. The mixture was poured into ice-cold water, adjusted to pH 10.5 with 40% aqueous potassium carbonate, and stirred under ice-cooling for 30 minutes. The mixture was extracted with a mixture of tetrahydrofuran and ethyl acetate 6 times. The organic layer was dried over magnesium sulfate and evaporated in vacuo to give 1-(2-hydroxyethyl)-5-formamidopyrazole (30.8 g).

後処理

  1. stirringthe mixture was stirred under ice-
  2. temperaturecooling for 30 minutes
  3. additionThe mixture was poured into ice-cold water
  4. stirringstirred under ice-
  5. temperaturecooling for 30 minutes
  6. extractionThe mixture was extracted with a mixture of tetrahydrofuran and ethyl acetate 6 times
  7. dry with materialThe organic layer was dried over magnesium sulfate
  8. customevaporated in vacuo

出典と根拠

ORDレコード
ord-a11476a6a9584ddf9f0ba0f5a727b73f
出典データセット
uspto-grants-1993_05
特許番号
US05210080

関連ノート

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