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Sodium Hydroxide → [1-(6-Chloropyridazin-3-yl)-3-methyl-5-phenyl-1H-pyrazol-4-yl]acetic acid

HRID 2068482
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HRID 2068482 반응식
[OH-].[Na+].C[O:4][C:5](=[O:26])[CH2:6][C:7]1[C:8]([CH3:25])=[N:9][N:10]([C:18]2[N:19]=[N:20][C:21]([Cl:24])=[CH:22][CH:23]=2)[C:11]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>CO>[Cl:24][C:21]1[N:20]=[N:19][C:18]([N:10]2[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[C:7]([CH2:6][C:5]([OH:26])=[O:4])[C:8]([CH3:25])=[N:9]2)=[CH:23][CH:22]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 131730043methyl[1-(6-chloropyridazin-3-yl)-3-methyl-5-phenyl-1H-pyrazol-4-yl]acetate

생성물 1

HCID 86642722[1-(6-Chloropyridazin-3-yl)-3-methyl-5-phenyl-1H-pyrazol-4-yl]acetic acid

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
20 °C

실험 절차

0.058 g (1.444 mmol) of 2-molar aqueous sodium hydroxide solution was added to 0.099 g (0.289 mmol) of methyl[1-(6-chloropyridazin-3-yl)-3-methyl-5-phenyl-1H-pyrazol-4-yl]acetate in 5.00 ml of methanol, and the mixture was stirred at 20° C. for 1 h. The methanol was removed under reduced pressure and the residue was poured into a mixture of 10 ml of water and 15 ml of dichloromethane. The aqueous phase was extracted with 15 ml of dichloromethane, acidified with concentrated hydrochloric acid (pH=3) and extracted three times with in each case 15 ml of dichloromethane. Drying of the combined organic phases and removal of the solvent under reduced pressure gave 0.052 g (54.7% of theory) of a brown wax-like solid.

후처리

  1. customThe methanol was removed under reduced pressure
  2. additionthe residue was poured into a mixture of 10 ml of water and 15 ml of dichloromethane
  3. extractionThe aqueous phase was extracted with 15 ml of dichloromethane
  4. extractionextracted three times with in each case 15 ml of dichloromethane
  5. customDrying of the combined organic phases and removal of the solvent under reduced pressure
  6. customgave 0.052 g (54.7% of theory) of a brown wax-like solid

출처 및 근거

ORD 기록
ord-d36ab2cede2943ae9d71b6046240b9b9
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08298994B2

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