Ammonia → Ethyl 5-(propan-2-yl)-1H-pyrazole-3-carboxylate

HRID 1827954노트

반응식

HRID 1827954 반응식
[CH:1]([C:4]1[NH:8][N:7]=[C:6]([C:9]([OH:11])=[O:10])[CH:5]=1)([CH3:3])[CH3:2].O.N.[CH2:14](O)[CH3:15]>S(=O)(=O)(O)O>[CH2:14]([O:10][C:9]([C:6]1[CH:5]=[C:4]([CH:1]([CH3:3])[CH3:2])[NH:8][N:7]=1)=[O:11])[CH3:15]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 702EthanolHCID 962WaterHCID 7764215-(propan-2-yl)-1H-pyrazole-3-carboxylic acid

생성물 1

HCID 6422484Ethyl 5-(propan-2-yl)-1H-pyrazole-3-carboxylate

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

5-Isopropyl-1H-pyrazole-3-carboxylic acid (WO 03/035065, page. 485, example 17b) (1.00 g, 6.49 mmol) was dissolved in a mixture of concentrated sulphuric acid (1.5 mL) and ethanol (25 mL) and the reaction mixture heated at reflux for 3 hours. The reaction mixture was cooled, poured into water, basified with 0.88 ammonia then extracted with ethyl acetate. The ethyl acetate was washed with brine, dried over magnesium sulphate and concentrated in vacuo to yield the title product, 514 mg (43%).

후처리

  1. temperaturethe reaction mixture heated
  2. temperatureat reflux for 3 hours
  3. temperatureThe reaction mixture was cooled
  4. extractionthen extracted with ethyl acetate
  5. washThe ethyl acetate was washed with brine
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5456da4cd07443dd9ae26f4f0434d1ff
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07056934B2

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