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

HRID 1485413노트

반응식

HRID 1485413 반응식
[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

참가 물질

4

반응물 2

HCID 14039AcetohydrazideHCID 303360874389-71-2

생성물 1

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

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5c2a6ecb2761459d8a570616bf93ab3e
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422292B2

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