Hydrazine hydrate (1:1) → 4-(4-chloro-3-methylphenyl)-1H-pyrazole-3,5-diamine

HRID 1912899노트

반응식

HRID 1912899 반응식
O.[NH2:2][NH2:3].[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([CH:11]([C:14]#[N:15])[C:12]#[N:13])=[CH:7][C:6]=1[CH3:16]>C(Cl)(Cl)Cl>[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:14]([NH2:15])=[N:2][NH:3][C:12]=2[NH2:13])=[CH:7][C:6]=1[CH3:16]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 866651792-(4-Chloro-3-methylphenyl)malononitrile

생성물 1

HCID 687511524-(4-chloro-3-methylphenyl)-1H-pyrazole-3,5-diamine

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
70 °C

실험 절차

Hydrazine monohydrate (0.312 mL, 6.4 mmol) was added to a solution of the product from Example 47A (512 mg, 2.69 mmol) in CHCl3 (25 mL). The reaction flask was evacuated and purged with nitrogen (3 cycles) and the mixture was heated at 70° C. under nitrogen for 22 hours, then cooled to room temperature. The mixture was concentrated under vacuum to provide the title compound as a beige solid. MS (DCI/NH3) m/z 223/225 (M+H)+.

후처리

  1. customThe reaction flask was evacuated
  2. custompurged with nitrogen (3 cycles)
  3. temperaturecooled to room temperature
  4. concentrationThe mixture was concentrated under vacuum

출처 및 근거

ORD 기록
ord-a4e073b01ed3423fab9e38b75e8a600e
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609669B2

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