Carbon Dioxide → 1-Hydroxypyrazole-4-carboxylic acid

HRID 622186ノート

反応式

HRID 622186 の反応式
[OH:1][N:2]1[CH:6]=[CH:5][CH:4]=[N:3]1.[C:7](=O)([O-:9])[O-:8].[K+].[K+].C(=O)=O.Cl>O>[OH:1][N:2]1[CH:6]=[C:5]([C:7]([OH:9])=[O:8])[CH:4]=[N:3]1

参加物

6

反応物 4

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 30167331-hydroxy-1H-pyrazole

生成物 1

HCID 137994111-Hydroxypyrazole-4-carboxylic acid収率 45%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1 part of 1-hydroxypyrazole is mixed thoroughly with 4 parts of potassium carbonate, and the mixture is introduced into an autoclave. Carbon dioxide is forced in at room temperature until the pressure reaches 50 bar, after which heating is carried out for 20 hours at 150° C. The reactor content is then dissolved in water, the solution is acidified with hydrochloric acid, which precipitates the 1-hydroxypyrazole-4-carboxylic acid, and the latter is filtered off and recrystallized from water. 0.68 part (45% of theory) of 1-hydroxypyrazole-4-carboxylic acid of melting point 230° C. is obtained.

後処理

  1. additionthe mixture is introduced into an autoclave
  2. customis forced in at room temperature until the pressure
  3. temperatureafter which heating
  4. customprecipitates the 1-hydroxypyrazole-4-carboxylic acid
  5. filtrationthe latter is filtered off
  6. customrecrystallized from water

出典と根拠

ORDレコード
ord-7f6b44bf592f4323965e02e0a99ba42f
出典データセット
uspto-grants-1988_09
特許番号
US04769473

反応ノート

読み込み中…