1-Aminocyclohexanecarboxylic acid → Methyl 1-aminocyclohexane-1-carboxylate hydrochloride

HRID 244068

反応式

HRID 244068 の反応式
[NH2:1][C:2]1([C:8]([OH:10])=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.S(Cl)([Cl:13])=O.[CH3:15]COCC>CO>[ClH:13].[NH2:1][C:2]1([C:8]([O:10][CH3:15])=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1

参加物

5

反応物 3

HCID 13661-Aminocyclohexanecarboxylic acidHCID 3283Diethyl EtherHCID 24386Thionyl Chloride

生成物 1

HCID 22645079Methyl 1-aminocyclohexane-1-carboxylate hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a suspension of 2 g (14 mmol) of 1-aminocyclohexanecarboxylic acid in 20 mL of methanol is sparged hydrogen chloride for 2 minutes. 1.2 mL (16.8 mmol) of thionyl chloride are added to the solution obtained and the reaction medium is refluxed for 6 hours. After cooling, the mixture is concentrated under reduced pressure and the residue obtained is taken up in 5 mL of methanol. 50 mL of ether are added so as to precipitate 2.3 g of methyl 1-aminocyclohexanecarboxylate hydrochloride in the form of a white powder.

後処理

  1. customis sparged hydrogen chloride for 2 minutes
  2. customobtained
  3. temperaturethe reaction medium is refluxed for 6 hours
  4. temperatureAfter cooling
  5. concentrationthe mixture is concentrated under reduced pressure
  6. customthe residue obtained
  7. customto precipitate 2.3 g of methyl 1-aminocyclohexanecarboxylate hydrochloride in the form of a white powder

出典と根拠

ORDレコード
ord-4e12714f91244160b488a881e4366428
出典データセット
uspto-grants-2014_02
特許番号
US08653276B2

関連ノート

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