Benzaldehyde → Methyl 2-benzylideneaminohexanoate

HRID 970304

반응식

HRID 970304 반응식
Cl.[NH2:2][CH:3]([CH2:8][CH2:9][CH2:10][CH3:11])[C:4]([O:6][CH3:7])=[O:5].C(N(CC)CC)C.S([O-])([O-])(=O)=O.[Mg+2].[CH:25](=O)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>ClCCl>[CH:25](=[N:2][CH:3]([CH2:8][CH2:9][CH2:10][CH3:11])[C:4]([O:6][CH3:7])=[O:5])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

참가 물질

6

반응물 4

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 14039064Methyl norleucinate--hydrogen chloride (1/1)

생성물 1

HCID 23074255Methyl 2-benzylideneaminohexanoate수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 7.79 g of methyl 2-aminohexanoate hydrochloride in 70 ml of dichloromethane were added 8.67 g of triethylamine (manufactured by WAKO PURE CHEMICAL INDUSTRIES LTD.), 7.74 g of anhydrous magnesium sulfate, and 4.55 g of benzaldehyde and the resultant was stirred overnight at room temperature. The reaction suspension was then filtered and the filtrate was concentrated. 280 ml of ether was added to the residue and the resultant suspension was filtered and the filtrate was concentrated. Again, 280 ml of ether was added to the residue and filtration and concentration were similarly repeated to obtain 10.0 g of the title compound.

후처리

  1. filtrationThe reaction suspension was then filtered
  2. concentrationthe filtrate was concentrated
  3. addition280 ml of ether was added to the residue
  4. filtrationthe resultant suspension was filtered
  5. concentrationthe filtrate was concentrated
  6. additionAgain, 280 ml of ether was added to the residue and filtration and concentration

출처 및 근거

ORD 기록
ord-332311d18c5f4149a4c880390161ac35
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07312208B2

연결된 노트

불러오는 중…