Hydrazine hydrate (1:1) → HCID 18763424、化合物

HRID 431382ノート

反応式

HRID 431382 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][C:21]=1[Cl:22])[O:5][CH2:6][C:7]1[CH:8]=[C:9]([N+:16]([O-])=O)[CH:10]=[C:11]([N+:13]([O-])=O)[CH:12]=1.O.NN>CO.[Ni]>[Cl:1][C:2]1[CH:3]=[C:4]([CH:19]=[CH:20][C:21]=1[Cl:22])[O:5][CH2:6][C:7]1[CH:8]=[C:9]([NH2:16])[CH:10]=[C:11]([NH2:13])[CH:12]=1

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 187634315-(3,4-Dichlorophenoxymethyl)-1,3-dinitrobenzene

生成物 1

HCID 18763424HCID 18763424、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

5-(3,4-dichlorophenoxymethyl)-1,3-dinitrobenzene in 5 ml MeOH was added to a solution of 10 ml 2.5 mmole hydrazine monohydrate and catalytic amount of Ra—Ni. The mixture was stirred under reflux for 30 min and then cooled to room temperature. GC-MS gave the peak of reduced product. The solution was filtered through Celite and MeOH was evaporated with rotaevaporation. The residue was used directly for next step without further purification.

後処理

  1. temperatureunder reflux for 30 min
  2. customGC-MS gave the peak of reduced product
  3. filtrationThe solution was filtered through Celite and MeOH
  4. customwas evaporated with rotaevaporation
  5. customThe residue was used directly for next step without further purification

出典と根拠

ORDレコード
ord-c09c85f942a7469e92ec2d9fdf50c5f7
出典データセット
uspto-grants-2003_12
特許番号
US06656971B2

反応ノート

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