Benzylamine → HCID 429236, 화합물

HRID 905120노트

반응식

HRID 905120 반응식
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH:10]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:11]([O:13][CH2:14][CH3:15])=[O:12]>C1C=CC=CC=1>[CH2:1]([NH:8][CH:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 7504BenzylamineHCID 69637Diethyl bromomalonate

생성물 1

HCID 429236HCID 429236, 화합물수율 21%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

Benzylamine (18.3 g) and diethyl bromomalonate (20.3 g) were dissolved in dry benzene (100 ml), and the mixture was heated under reflux for 14 hours with stirring. The precipitated salt was removed by filtration from the reaction mixture. The filtrate was washed with dilute hydrochloric acid to remove the unreacted benzylamine. The benzene layer was washed with water three times, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography using hexane/ethyl acetate (4:1) as an eluent to give 4.7 g (yield 21%) of diethyl benzylaminomalonate having the following NMR data.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 14 hours
  3. customThe precipitated salt was removed by filtration from the reaction mixture
  4. washThe filtrate was washed with dilute hydrochloric acid
  5. customto remove the unreacted benzylamine
  6. washThe benzene layer was washed with water three times
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off under reduced pressure
  9. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-0c5afdae08b6483ab92970860bcc30e2
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04421914

반응 노트

불러오는 중…