Water → Ethyldiisopropylethylamine

HRID 374668노트

반응식

HRID 374668 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 109972602-(Diisopropylamino)propionitrileHCID 178418443HCID 178418443, 화합물

생성물 1

HCID 18997630Ethyldiisopropylethylamine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c0d7bf166159428fb422e6c482e76f6a
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05481038

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