Methanol → Methyl 12-aminododecanoate

HRID 1291689

反応式

HRID 1291689 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 3665980Methyl 12-aminododecanoate収率 95%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
60 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-65d1920ed434425f8e8e578931e129a0
出典データセット
uspto-grants-1998_05
特許番号
US05753707

関連ノート

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