4-Nitrobenzaldehyde → HCID 18472662, 화합물

HRID 566062

반응식

HRID 566062 반응식
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH:8]=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].Cl.[CH3:13][O:14][C:15](=[O:19])[CH2:16][NH:17][CH3:18].C(N(CC)CC)C.O>ClCCCl>[CH3:13][O:14][C:15](=[O:19])[CH2:16][N:17]([CH2:8][C:7]1[CH:10]=[CH:11][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)[CH3:18]

참가 물질

6

반응물 4

HCID 5414-NitrobenzaldehydeHCID 962WaterHCID 8471TriethylamineHCID 83544Glycine, N-methyl-, methyl ester, hydrochloride (1:1)

생성물 1

HCID 18472662HCID 18472662, 화합물수율 80.2%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

In 1,2-dichloroethane (50 ml) were suspended p-nitrobenzaldehyde (5 g), sarcosine methyl ester hydrochloride (4.6 g) and triethylamine (4.6 ml), and to the mixture was added, under ice-cooling, triacetoxy sodium boron hydride (9.8 g). Under nitrogen atmosphere, the mixture was stirred at room temperature for 4 hours. To the mixture was added water, and the mixture was concentrated, neutralized with sodium hydroxide solution and extracted with ethyl acetate. The organic layer was washed with water and brine, and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column (ethyl acetate/hexane) to give N-(4-nitrobenzyl)sarcosine methyl ester (6.3 g) as colorless oil.

후처리

  1. additionto the mixture was added, under ice-
  2. temperaturecooling
  3. concentrationthe mixture was concentrated
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with water and brine
  6. dry with materialdried with anhydrous magnesium sulfate
  7. customUnder reduced pressure, the solvent was evaporated
  8. customthe residue was purified with silica gel column (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-ec5112c45ac9435d8695ad166943129b
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06172061B2

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