Ethyl Acetate → HCID 178507285、化合物

HRID 1695192ノート

反応式

HRID 1695192 の反応式
[NH2:1][C:2]1[CH:6]=[CH:5][NH:4][N:3]=1.CCO[C:10]([CH3:12])=O>>[N:1]1[CH:12]=[CH:10][CH:5]=[CH:6][C:2]=1[C:5]1[CH:6]=[C:2]([NH2:1])[NH:3][N:4]=1

参加物

3

反応物 2

HCID 8857Ethyl AcetateHCID 178418806HCID 178418806、化合物

生成物 1

HCID 178507285HCID 178507285、化合物収率 60%

反応条件

温度
80 °C

実験手順

The product was prepared according to general procedure for aminopyrazole synthesis (route A2). The crude product was dissolved in EtOAc, washed with NaHCO3, dried and evaporated. NMR analysis showed that a major portion of the crude mixture was still in the opened form: the mixture was then dissolved in CH3COOH and heated at 80° C. overnight, to allow for ring closure of the opened form. The product was then recovered as the acylated form, which was de-acylated stirring with HCl 6N at 60° C. overnight obtaining the title product (0.816 g, yield 60%).

後処理

  1. customThe product was prepared
  2. washwashed with NaHCO3
  3. customdried
  4. customevaporated
  5. dissolutionthe mixture was then dissolved in CH3COOH
  6. customThe product was then recovered as the acylated form, which

出典と根拠

ORDレコード
ord-e1e270f83c994c5abcdef3e8f8684f46
出典データセット
uspto-grants-2012_04
特許番号
US08163729B2

反応ノート

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