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2-Propanone, 1-nitro- → HCID 54296870, 화합물

HRID 1110345
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HRID 1110345 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([CH:13]=[CH:14][CH:15]=1)[CH:7]=NCCCC)([O-:3])=[O:2].[N+:16]([CH2:19][C:20](=[O:22])[CH3:21])([O-:18])=[O:17]>C(OC(=O)C)(=O)C>[N+:1]([C:4]1[CH:5]=[C:6]([CH:7]=[C:19]([N+:16]([O-:18])=[O:17])[C:20](=[O:22])[CH3:21])[CH:13]=[CH:14][CH:15]=1)([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 662962-Propanone, 1-nitro-HCID 14971160(E)-N-Butyl-1-(3-nitrophenyl)methanimine

생성물 1

HCID 54296870HCID 54296870, 화합물수율 27.1%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

To a solution of 28.6 g (0.39 mole) of the butanamine in 75 mL of acetic anhydride was added 15 g of 1-nitro-2-propanone. A white precipitate formed almost at once. The mixture was warmed gently until the solid dissolved, cooled, stirred for five hours, carefully poured onto water and extracted with ether. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate and the solvent removed under reduced pressure. After storage at 0° C. overnight, the residue had crystallized. Recrystallization of the resulting solid from dibutyl ether gave 9.3 g of 4-(3-nitrophenyl)-3-nitro-3-buten-2-one, 1H NMR 8.4 (m, 2H), 7.7 (m, 2H), 7.5 (s, 1H), 2.5 (s, 3H).

후처리

  1. customA white precipitate formed almost at once
  2. temperatureThe mixture was warmed gently until the solid
  3. dissolutiondissolved
  4. temperaturecooled
  5. additioncarefully poured onto water
  6. extractionextracted with ether
  7. customThe organic layer was separated
  8. washwashed with water
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customthe solvent removed under reduced pressure
  11. customAfter storage at 0° C. overnight, the residue had crystallized
  12. customRecrystallization of the resulting solid from dibutyl ether

출처 및 근거

ORD 기록
ord-c16a7a3e194648138e26583ea2eb4028
출처 데이터셋
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04975437

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