Diethyl Ether → Ethyl 2-Aminobutyrate Hydrochloride

HRID 848

反応式

HRID 848 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 (120.8 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. stirringwith hand stirring
  8. filtrationThe suspension was filtered
  9. customthe solid product dried

出典と根拠

ORDレコード
ord-57d496f8cfa74e14b0b60ed9b08a5969
出典データセット
uspto-grants-1998_03
特許番号
US05723458

関連ノート

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