Water → Ethyldiisopropylethylamine

HRID 374668ノート

反応式

HRID 374668 の反応式
[CH:1]([N:4]([CH:9]([CH3:11])[CH3:10])[CH:5]([CH3:8])[C:6]#N)([CH3:3])[CH3:2].[CH2:12]([Mg]Br)C.O>C(OCC)C>[CH:1]([N:4]([CH:5]([CH2:6][CH3:12])[CH3:8])[CH:9]([CH3:11])[CH3:10])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 962WaterHCID 109972602-(Diisopropylamino)propionitrileHCID 178418443HCID 178418443、化合物

生成物 1

HCID 18997630Ethyldiisopropylethylamine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of 2-(diisopropylamino)propionitrile (25.00 g, 0.162 mol) in diethyl ether (20 ml) was added dropwise to a 1M solution of ethyl magnesium bromide in diethyl ether (32.4 ml, 0.324 mol) and the mixture was refluxed for 30 min. Water (25 ml) was added and white precipitate was filtered off and washed with diethyl ether (2×100 ml). The ether solutions were combined, dried over anhydrous magnesium sulfate and the product was isolated by distillation: 13.80 g, 51%, bp 60°-62° C./20 mm Hg. 1H NMR CDCl3 δ ppm, 0.85 (t, J=6.5 Hz, 3H, CH3) , 0.98 (d, J=6.5 Hz, 6H, CH3) 0.99 (d, J=6.5 Hz, 3H, CH3), 1.05 (d, J=6.5 Hz, 6H, CH3) , 1.17-1.44(m, 2H, CH2), 2.70 (m, 1H, CH), 3.08 (sep, J=6.5 Hz, 2H, CH).

後処理

  1. temperaturethe mixture was refluxed for 30 min
  2. filtrationwhite precipitate was filtered off
  3. washwashed with diethyl ether (2×100 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe product was isolated by distillation

出典と根拠

ORDレコード
ord-c0d7bf166159428fb422e6c482e76f6a
出典データセット
uspto-grants-1996_01
特許番号
US05481038

反応ノート

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