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

HRID 1912899ノート

反応式

HRID 1912899 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
70 °C

実験手順

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)+.

後処理

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

出典と根拠

ORDレコード
ord-a4e073b01ed3423fab9e38b75e8a600e
出典データセット
uspto-grants-2013_12
特許番号
US08609669B2

反応ノート

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