Potassium Nitrate → 10-Methyl-7-nitro-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H,11aH)-dione

HRID 369948

반응식

HRID 369948 반응식
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:6](=[O:13])[N:5]2[CH2:14][CH2:15][CH2:16][CH:4]2[C:3]1=[O:17].[N+:18]([O-])([O-:20])=[O:19].[K+]>S(=O)(=O)(O)O>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][C:11]([N+:18]([O-:20])=[O:19])=[CH:12][C:7]=2[C:6](=[O:13])[N:5]2[CH2:14][CH2:15][CH2:16][CH:4]2[C:3]1=[O:17]

참가 물질

4

반응물 2

HCID 24434Potassium NitrateHCID 985943610-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H,11aH)-dione

생성물 1

HCID 7013377410-Methyl-7-nitro-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H,11aH)-dione

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To 10-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H,11aH)-dione (5.7 g, 24.7 mmol) in concentrated sulfuric acid (60 ml) at 0° C. was added potassium nitrate (2.62 g, 25.9 mmol). After stirring for 2 h the mixture was dumped onto ice (500 g) and extracted with ethyl acetate (5×75 ml). The combined extracts were washed with water, dried over magnesium sulfate, filtered, and concentrated to a solid which was recrystallized from ethyl acetate-hexane (5.2 g, 77%), m.p. 160-162° C.

후처리

  1. extractionextracted with ethyl acetate (5×75 ml)
  2. washThe combined extracts were washed with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to a solid which
  6. customwas recrystallized from ethyl acetate-hexane (5.2 g, 77%), m.p. 160-162° C.

출처 및 근거

ORD 기록
ord-8635e32687494b0d920640d321ee7743
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06140322

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