Methanol → Methyl 12-aminododecanoate

HRID 1291689

반응식

HRID 1291689 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([OH:15])=[O:14].CO.S(=O)(=O)(O)O.[C:23](=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl>[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH3:23])=[O:14]

참가 물질

6

반응물 4

HCID 887MethanolHCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 6966112-Aminododecanoic Acid

생성물 1

HCID 3665980Methyl 12-aminododecanoate수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
60 °C

실험 절차

To a 3-l flask equipped with a stirrer, 200.0 g (0.93 mol) of 12-aminododecanoic acid, 600 g of methanol and 100 g (1.0 mol) of sulfuric acid were charged, followed by stirring at 60° C. for 5 hours. After the reaction mixture was allowed to cool down, it was diluted with methylene chloride, followed by neutralization with an aqueous solution of sodium carbonate. The solvent was distilled off under reduced pressure, followed by purification by chromatography on an alumina short column, whereby 201.7 g of the title compound (7-a) were obtained (yield: 95%).

후처리

  1. customTo a 3-l flask equipped with a stirrer
  2. temperatureto cool down
  3. distillationThe solvent was distilled off under reduced pressure
  4. customfollowed by purification by chromatography on an alumina short column

출처 및 근거

ORD 기록
ord-65d1920ed434425f8e8e578931e129a0
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753707

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