Methylhydrazine → 5-Amino-1-methyl-4-nitroso-3-phenylpyrazole

HRID 1085159ノート

反応式

HRID 1085159 の反応式
[OH:1][N:2]=[C:3]([C:6](=O)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:4]#[N:5].[CH3:14][NH:15][NH2:16]>C(O)C>[NH2:5][C:4]1[N:15]([CH3:14])[N:16]=[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:3]=1[N:2]=[O:1]

参加物

4

反応物 2

HCID 6061MethylhydrazineHCID 85446889HCID 85446889、化合物

生成物 1

HCID 53253435-Amino-1-methyl-4-nitroso-3-phenylpyrazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-hydroxyimino-3-oxo-3-phenylpropanenitrile (2.61 g, 15 mmol) and methylhydrazine (1.1 ml, 21 mmol) was stirred at reflux in ethanol (20 ml) for 2 hours, cooled and concentrated under reduced pressure. The residue was partitioned between ether (50 ml) and dilute hydrochloric acid (50 ml, 2N solution). The aqueous phase was separated and rendered basic by the addition of saturated aqueous potassium carbonate. The red solid which precipitated was filtered off and dried, to give the title compound, 1.40 g, (46%). m.p. 230°-231° C. (literature. m.p. 230°-231° C., Gazz. Chim. Ital., (1968), 98, 569.

後処理

  1. temperaturecooled
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was partitioned between ether (50 ml) and dilute hydrochloric acid (50 ml, 2N solution)
  4. customThe aqueous phase was separated
  5. additionrendered basic by the addition of saturated aqueous potassium carbonate
  6. customThe red solid which precipitated
  7. filtrationwas filtered off
  8. customdried

出典と根拠

ORDレコード
ord-15125575561b426caee623cc83c08b6c
出典データセット
uspto-grants-1991_04
特許番号
US05008263

反応ノート

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