Benzene → Morpholine, 4-(6-hydrazinyl-3-pyridazinyl)-, hydrochloride (1:2)

HRID 1065483ノート

反応式

HRID 1065483 の反応式
[N+](C1C=CC(C=[N:9][NH:10][C:11]2[N:12]=[N:13][C:14]([N:17]3[CH2:22][CH2:21][O:20][CH2:19][CH2:18]3)=[CH:15][CH:16]=2)=CC=1)([O-])=O.C1C=CC=CC=1.C1(C)C=CC=CC=1.[Cl:38]CCl>C(Cl)(Cl)Cl>[ClH:38].[ClH:38].[O:20]1[CH2:21][CH2:22][N:17]([C:14]2[N:13]=[N:12][C:11]([NH:10][NH2:9])=[CH:16][CH:15]=2)[CH2:18][CH2:19]1

参加物

6

反応物 4

HCID 241BenzeneHCID 1140TolueneHCID 6344DichloromethaneHCID 70550960HCID 70550960、化合物2 回

生成物 1

HCID 12603549Morpholine, 4-(6-hydrazinyl-3-pyridazinyl)-, hydrochloride (1:2)

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
40 °C

実験手順

One part by weight of the substituted benzylidenehydrazine (compounds of Examples 1 to 6) is heated together with 20 parts by volume of benzene (or toluene or dichloromethane or chloroform) and 20 parts by volume of concentrated hydrochloric (or 48% hydrobromic) acid while stirring at an internal temperature of 40° C. for 1 to 2 hours in such a way that the organic phase is replaced by fresh solvent every 30 minutes. After separation 80-90% of the substituted benzaldehyde can be recovered from the organic phase. From the acidic aqueous phase, 6-morpholino-3-pyridazinylhydrazine dihydrochloride (or dihydrobromide, respectively) is obtained after evaporation and triturating the residue with ethanol and ether.

後処理

  1. waitis replaced by fresh solvent every 30 minutes
  2. customAfter separation 80-90% of the substituted benzaldehyde
  3. customcan be recovered from the organic phase

出典と根拠

ORDレコード
ord-d7f74f1af61c4b3091cbfcff9e9b89be
出典データセット
uspto-grants-1982_05
特許番号
US04329457

反応ノート

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