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

HRID 1827954ノート

反応式

HRID 1827954 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-5456da4cd07443dd9ae26f4f0434d1ff
出典データセット
uspto-grants-2006_06
特許番号
US07056934B2

反応ノート

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