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

HRID 1085159노트

반응식

HRID 1085159 반응식
[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]

참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 85446889HCID 85446889, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-15125575561b426caee623cc83c08b6c
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05008263

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