Water → 4-(Morpholin-4-yl)butan-1-amine

HRID 924628

반응식

HRID 924628 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[N:7]1([CH2:13][CH2:14][CH2:15][C:16]#[N:17])[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1.O>CCOCC>[N:7]1([CH2:13][CH2:14][CH2:15][CH2:16][NH2:17])[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1

참가 물질

5

반응물 3

HCID 962WaterHCID 2945744-MorpholinebutanenitrileHCID 21226445Aluminium lithium hydride

생성물 1

HCID 2336114-(Morpholin-4-yl)butan-1-amine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

반응 조건

온도
-55 °C

실험 절차

14.8 g lithium aluminium hydride were weighed under N2 atmosphere into a round-bottomed flask. The substance was cooled down to −55° C. and 150 ml ether was added dropwise. The suspension was allowed to stir; then 30 g 4-Morpholin-4-yl-butyronitrile were dissolved in 200 ml ether and the solution was added dropwise to the reaction mixture. Again 200 ml ether were added to the mixture and the reaction was stirred at room temperature overnight. At the next day the mixture was cooled down to less than 10° C. and 35 ml H2O were added carefully. After five hours the mixture was fritted and the residue was washed with 300 ml ether. The filtrate was dried, concentrated and finally distilled under vacuum. The product fractions were collected at 74-78° C. and 2.1-1.6 Torr. The purity of the colourless oil was judged by gas chromatography, GC-MS and 1H-NMR.

후처리

  1. additionthe solution was added dropwise to the reaction mixture
  2. stirringthe reaction was stirred at room temperature overnight
  3. temperatureAt the next day the mixture was cooled down to less than 10° C.
  4. washthe residue was washed with 300 ml ether
  5. customThe filtrate was dried
  6. concentrationconcentrated
  7. distillationfinally distilled under vacuum
  8. customThe product fractions were collected at 74-78° C.

출처 및 근거

ORD 기록
ord-92f7a95456c54f34bfec5a34c62b39ec
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09283186B2

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