Acetamide → N-Acetyl-1,6-diaminohexane

反応式

[NH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH2:8].[C:9](N)(=[O:11])[CH3:10]>>[C:9]([NH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][NH2:8])(=[O:11])[CH3:10]

参加物

反応物 2

HCID 178Acetamide

HCID 16402Hexamethylenediamine

生成物 1

HCID 162081N-Acetyl-1,6-diaminohexane

実験手順

Hexamethylenediamine (90.64 g; 0.6 mol) and acetamide (11.81 g; 0.2 Mol) were stirred and refluxed for 10 hours under nitrogen. The solution was cooled overnight and then distilled under vacuum <100° C. as fast as possible. The N-acetylhexylenediamine was then separated from the resultant mixture by flash chromatography [SiO2/EtOH:25%aq.NH3 (4:1)]. The title product was obtained as a white crystalline product (18.43 g; 58% theory).

後処理

temperaturerefluxed for 10 hours under nitrogen
temperatureThe solution was cooled overnight
distillationdistilled under vacuum <100° C. as fast as possible
customThe N-acetylhexylenediamine was then separated from the resultant mixture by flash chromatography [SiO2/EtOH:25%aq.NH3 (4:1)]

出典と根拠

ORDレコード: ord-35c5df770b194cc5a9ffc293550b73f2
出典データセット: uspto-grants-2004_03
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06706855B1

反応ノート

読み込み中…

参加物