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2-Propanone, 1-nitro- → HCID 54296870、化合物

HRID 1110345
ノート
印刷プレビュー

反応式

HRID 1110345 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 54296870HCID 54296870、化合物収率 27.1%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c16a7a3e194648138e26583ea2eb4028
出典データセット
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04975437

反応ノート

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