Methylhydrazine → 2,4,5,6-Tetrahydro-2-methyl-6-(4-nitrobenzoyl)-pyrazolo[4,3-d][1]benzazepin

HRID 355869

반응식

HRID 355869 반응식
[CH3:1][N:2]([CH:4]=[C:5]1[C:11](=O)[C:10]2[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=2[N:8]([C:17](=[O:27])[C:18]2[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=2)[CH2:7][CH2:6]1)C.C[NH:29]N>CO>[CH3:1][N:2]1[CH:4]=[C:5]2[CH2:6][CH2:7][N:8]([C:17](=[O:27])[C:18]3[CH:19]=[CH:20][C:21]([N+:24]([O-:26])=[O:25])=[CH:22][CH:23]=3)[C:9]3[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=3[C:11]2=[N:29]1

참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 536535644-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one

생성물 1

HCID 571133932,4,5,6-Tetrahydro-2-methyl-6-(4-nitrobenzoyl)-pyrazolo[4,3-d][1]benzazepin

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 0.150 g of 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one and 44 μl of methylhydrazine in 5 ml of methyl alcohol is heated at reflux for 18 hours. A precipitate forms on standing. The volatiles are evaporated to a residue which is purified by column chromatography on silica gel by elution with 5% ethyl acetate-methylene chloride. The product fractions are combined and the volatiles evaporated to a residue which is dissolved in chloroform-methanol, filtered through glass wool and the filtrate evaporated in vacuo to give 0.110 g of the desired product as pale yellow crystals.

후처리

  1. temperatureat reflux for 18 hours
  2. customThe volatiles are evaporated to a residue which
  3. customis purified by column chromatography on silica gel by elution with 5% ethyl acetate-methylene chloride
  4. customthe volatiles evaporated to a residue which
  5. dissolutionis dissolved in chloroform-methanol
  6. filtrationfiltered through glass wool
  7. customthe filtrate evaporated in vacuo

출처 및 근거

ORD 기록
ord-f2441699a4154e82a18ddbb00b69d577
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05834461

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