反応式
O[CH:2]1C(=C)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=O.[C:13]([O-:16])(=O)[CH3:14].[NH4+:17]>C(O)C>[NH2:17][CH:2]=[C:3]1[CH2:4][C:5]2[C:14](=[CH:9][CH:8]=[CH:7][CH:6]=2)[C:13]1=[O:16]参加物
実験手順
To a stirred solution of 2-hydroxy-methylene-1-indanone (1.6 kg. as a 3.7 kg. wet cake) dissolved in ethanol (30 liters), and under a nitrogen atmosphere was added ammonium acetate (1.92 kg. 24.8 mole). After eight hours the reaction was complete and the ethanol was removed by vacuum distillation. The reaction mixture was cooled to room temperature and after filtration and air drying (1 hr.) yielded crude 2-aminomethylene-1-indanone (I) as orange crystals. The crystals were then dissolved in a minimum amount of hot ethanol and the solution was decolorized with activated charcoal. Crystals appeared in the filtrate and after cooling overnight at 5° C, the reaction mixture was filtered yielding 960 gm. of compound (I) as light orange crystals. The filtrate was again treated with activated charcoal and recrystallized providing an additional 200 gm. of compound (I). The combined sample (1160 gm.) was milled giving a fine yellowish powder which was dried at 50° C/25 mm/Hg for 48 hours. A sample (50 gm.) of this material was recrystallized three times from ethanol to give 2-aminomethylene-1-indanone (15 gm.), m.p. 166°-168° C.
後処理
- customthe ethanol was removed by vacuum distillation
- filtrationafter filtration and air
- customdrying (1 hr.)
出典と根拠
- ORDレコード
- ord-c0e3065d575b45bd855dd63e2ea02164
- 出典データセット
- uspto-grants-1977_12
- 特許番号
- US04064272
関連ノート
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