Methylhydrazine → HCID 14126711、化合物

HRID 569917ノート

反応式

HRID 569917 の反応式
[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

参加物

4

反応物 2

HCID 6061MethylhydrazineHCID 20146597HCID 20146597、化合物

生成物 1

HCID 14126711HCID 14126711、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-49b5eef246c543ec9dc76b48c7c61ebf
出典データセット
uspto-grants-1988_03
特許番号
US04734430

反応ノート

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