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

HRID 1065483노트

반응식

HRID 1065483 반응식
[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

참가 물질

6

반응물 4

HCID 241BenzeneHCID 1140TolueneHCID 6344DichloromethaneHCID 70550960HCID 70550960, 화합물2회

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d7f74f1af61c4b3091cbfcff9e9b89be
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04329457

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