Water → 2,2'-((Phenylmethyl)imino)bisethanol

HRID 895638

반응식

HRID 895638 반응식
[OH:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][OH:7].[CH2:8](Br)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[OH:1][CH2:2][CH2:3][N:4]([CH2:5][CH2:6][OH:7])[CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7498Benzyl BromideHCID 8113DiethanolamineHCID 11430Potassium Carbonate

생성물 1

HCID 75532,2'-((Phenylmethyl)imino)bisethanol수율 75%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Bis(2-hydroxyethyl)amine (5 g) was dissolved in N,N-dimethylformamide (100 ml), added with benzyl bromide (6.52 ml) and potassium carbonate (8.657 g) and stirred at room temperature for 21 hours. The reaction mixture was added with water (200 ml) and extracted twice with dichloromethane (200 ml). The organic layer was dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: dichloromethane:methanol=20:1→10:1) to obtain 7.631 g of the title compound. Yield: 75%.

후처리

  1. extractionextracted twice with dichloromethane (200 ml)
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (elution solvent: dichloromethane:methanol=20:1→10:1)

출처 및 근거

ORD 기록
ord-7ac300001659493c86f922de99e4dc72
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06916822B2

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