Methylhydrazine → HCID 14126711, 화합물

HRID 569917노트

반응식

HRID 569917 반응식
[CH3:1][NH:2][NH2:3].[CH3:4][N:5]1[C:13]2[CH2:12][C:11]([CH3:15])([CH3:14])[CH:10]([CH:16]=O)[C:9](=O)[C:8]=2[CH:7]=[N:6]1>CO>[CH3:1][N:2]1[CH:16]=[C:10]2[C:11]([CH3:15])([CH3:14])[CH2:12][C:13]3[N:5]([CH3:4])[N:6]=[CH:7][C:8]=3[C:9]2=[N:3]1

참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 20146597HCID 20146597, 화합물

생성물 1

HCID 14126711HCID 14126711, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of 0.59 ml of methylhydrazine in 20 ml of methanol was added dropwise to an ice-cold solution of 2.2 g of 4,5,6,7-tetrahydro-1,6,6-trimethyl-4-oxo-1H-indazole-5-carboxaldehyde in 80 ml of methanol. The solution was heated at reflux for 45 minutes and the solvent was removed under reduced pressure. The residue was dissolved in hot toluene and cooled to provide off-white crystals which were recrystallized from toluene to give 2,4,5,6-tetrahydro-2,4,4,6-tetramethylbenzo[1,2-c:3,4-c']dipyrazole melting at about 172°-173° C. The initial toluene mother liquor was concentrated under reduced pressure to provide tan crystals which were recrystallized from toluene to give 1,4,5,6-tetrahydro-1,4,4,6-tetramethylbenzo[1,2-c:3,4-c']dipyrazole melting at about 105°-108° C.

후처리

  1. temperatureThe solution was heated
  2. temperatureat reflux for 45 minutes
  3. customthe solvent was removed under reduced pressure
  4. dissolutionThe residue was dissolved in hot toluene
  5. temperaturecooled
  6. customto provide off-white crystals which
  7. customwere recrystallized from toluene

출처 및 근거

ORD 기록
ord-49b5eef246c543ec9dc76b48c7c61ebf
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04734430

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