Diethyl Ether → Ethyl 2-benzylideneamino-2-ethylhexanoate

HRID 398810

반응식

HRID 398810 반응식
[H-].[Na+].[CH:3](=[N:10][CH:11]([CH2:17][CH3:18])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH2:19](I)[CH2:20]CC.[Cl-].[NH4+].[CH2:26](OCC)[CH3:27]>CN(C)C=O.O>[CH:3](=[N:10][C:11]([CH2:26][CH3:27])([CH2:17][CH2:18][CH2:19][CH3:20])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

8

반응물 5

HCID 3283Diethyl EtherHCID 10962Butyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 10331026Ethyl 2-benzylideneaminobutyrate

생성물 1

HCID 10107458Ethyl 2-benzylideneamino-2-ethylhexanoate

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매3회

실험 절차

Sodium hydride (32.5 g, 60% dispersion in oil) and N,N-dimethylformamide (DMF) (700 ml) were stirred under nitrogen at room temperature and a solution of the product from (b) (178.1 g) in DMF was added dropwise. After 2 hours stirring at room temperature, a solution of butyl iodide (149.5 g) in DMF was added dropwise and the reaction left stirring for a further 2 hours. The reaction was poured into an ice cold mixture of water (560 ml), diethyl ether (300 ml) and ammonium chloride (120 g). The resulting organic layer was dried over potassium carbonate then concentrated to give the desired product as a brown oil (220 g).

후처리

  1. waitthe reaction left
  2. stirringstirring for a further 2 hours
  3. dry with materialThe resulting organic layer was dried over potassium carbonate
  4. concentrationthen concentrated

출처 및 근거

ORD 기록
ord-67b80e9de909443fa754ebafe5ec1aa4
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05817652

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