Diethyl Ether → Ethyl 2-Aminobutyrate Hydrochloride

HRID 342859

反応式

HRID 342859 の反応式
[NH2:1][CH:2]([CH2:6][CH3:7])[C:3]([OH:5])=[O:4].S(Cl)([Cl:10])=O.[CH2:12](OCC)[CH3:13]>C(O)C>[ClH:10].[NH2:1][CH:2]([CH2:6][CH3:7])[C:3]([O:5][CH2:12][CH3:13])=[O:4]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 6657Alpha-Aminobutyric AcidHCID 24386Thionyl Chloride

生成物 1

HCID 12844023Ethyl 2-Aminobutyrate Hydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

A slurry of 2-aminobutyric acid (100 g, Aldrich) in absolute ethanol (300 ml) was stirred under nitrogen at 0° C. and thionyl chloride (120.79 g) was added dropwise. The reaction was stirred overnight at 0° C. and then gradually warmed to room temperature. The resulting white slurry was heated under reflux for 3 hours, left to cool for 10 minutes, then poured into chilled diethyl ether (600 ml) with hand stirring. The suspension was filtered and the solid product dried to give the desired product (150 g) as a white solid. 1H NMR consistent with proposed structure.

後処理

  1. temperaturegradually warmed to room temperature
  2. temperatureThe resulting white slurry was heated
  3. temperatureunder reflux for 3 hours
  4. waitleft
  5. temperatureto cool for 10 minutes
  6. additionpoured
  7. stirringstirring
  8. filtrationThe suspension was filtered
  9. customthe solid product dried

出典と根拠

ORDレコード
ord-ef69e2d14e8743fda5daeb2393372b0e
出典データセット
uspto-grants-1999_01
特許番号
US05859240

関連ノート

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