反応式
[CH3:1][N:2]([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH3:3].[Br:14][CH2:15][CH2:16][CH2:17][Cl:18].CO>CCCCCC.C(OC)(C)(C)C>[Br-:14].[Cl:18][CH2:17][CH2:16][CH2:15][N+:2]([CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])([CH3:1])[CH3:3]参加物
5
反応条件
- 温度
- 65 °C
実験手順
Into a 1000 mL, round-bottomed flask equipped with air condensers and a magnetic stirring plate was charged N,N-dimethyldecylamine (200.0 grams, 1.08 moles), 1-bromo-3-chloropropane (170 grams, 1.08 moles) and methanol (200 mL). The reaction was maintained at 65° C. for 18 hours. Solvent was removed by rotary evaporation under reduced pressure and furthermore with high vacuum distillation to yield brown oil. The oil was placed in a beaker and stirred with hexane/t-butylmethylether 1:1 solution (400 mL) causing a white precipitate. The solids were collected by vacuum filtration. Solids were dried in a vacuum oven at 30° C. overnight. Yield 305.0 grams (0.089 moles, 82%).
後処理
- customInto a 1000 mL, round-bottomed flask equipped with air condensers
- customSolvent was removed by rotary evaporation under reduced pressure and furthermore with high vacuum distillation
- customto yield brown oil
- filtrationThe solids were collected by vacuum filtration
- customSolids were dried in a vacuum oven at 30° C. overnight
出典と根拠
- ORDレコード
- ord-d1033feccafd4fd0af23433b4b7180af
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05969090
関連ノート
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