Acetohydrazide → 1,5-Dimethyl-5,6-dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine

HRID 1485413ノート

反応式

HRID 1485413 の反応式
[CH3:1][CH:2]1[CH2:8][C:7](=S)[NH:6][C:5]2[CH:10]=[CH:11][CH:12]=[CH:13][C:4]=2[NH:3]1.[C:14]([NH:17][NH2:18])(=O)[CH3:15]>CCCCO>[CH3:15][C:14]1[N:6]2[C:5]3[CH:10]=[CH:11][CH:12]=[CH:13][C:4]=3[NH:3][CH:2]([CH3:1])[CH2:8][C:7]2=[N:18][N:17]=1

参加物

4

反応物 2

HCID 14039AcetohydrazideHCID 303360874389-71-2

生成物 1

HCID 4000941,5-Dimethyl-5,6-dihydro-4H-[1,2,4]triazolo[4,3-a][1,5]benzodiazepine収率 45%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A solution of 4-methyl-4,5-dihydro-1H-benzo[b][1,4]diazepine-2(3H)-thione (200 mg, 1.04 mmol) and acetohydrazide (150 mg, 2.07 mmol) in n-BuOH (10 mL) was heated at 130° C. overnight. The reaction mixture was evaporated, and then water (10 mL) was added, extracted with ethyl acetate (10 mL), dried with Na2SO4, and concentrated to give the crude product, which was purified by prep-TLC to give 1,5-dimethyl-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepine (100 mg, 45%).

後処理

  1. customThe reaction mixture was evaporated
  2. additionwater (10 mL) was added
  3. extractionextracted with ethyl acetate (10 mL)
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated
  6. customto give the crude product, which
  7. customwas purified by prep-TLC

出典と根拠

ORDレコード
ord-5c2a6ecb2761459d8a570616bf93ab3e
出典データセット
uspto-grants-2016_08
特許番号
US09422292B2

反応ノート

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