Carbon Dioxide → 1-Hydroxypyrazole-4-carboxylic acid

HRID 622186노트

반응식

HRID 622186 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 137994111-Hydroxypyrazole-4-carboxylic acid수율 45%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7f6b44bf592f4323965e02e0a99ba42f
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04769473

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