Methyl propiolate → HCID 86681478、化合物

反応式

[NH2:1]/[C:2](/[CH3:9])=[CH:3]\[C:4]([O:6][CH2:7][CH3:8])=[O:5].[C:10]([O:14][CH3:15])(=[O:13])[C:11]#[CH:12]>>[NH2:1]/[C:2](=[C:3](\[C:4]([O:6][CH2:7][CH3:8])=[O:5])/[CH:12]=[CH:11]/[C:10]([O:14][CH3:15])=[O:13])/[CH3:9]

参加物

反応物 2

HCID 13536Methyl propiolate

HCID 6437562-Butenoic acid, 3-amino-, ethyl ester, (2Z)-

生成物 1

HCID 86681478HCID 86681478、化合物収率 93.8%

反応条件

温度: 110 °C

実験手順

Ethyl (2Z)-3-aminobut-2-enoate (6.46 g, 50.0 mmol) and methyl propiolate (4.20 g, 50.0 mmol) were mixed in one 100 mL flask, and the mixture was stirred at 110° C. for 10 hrs. The reaction mixture was cooled to room temperature and recrystallized with methanol to give 10 g (93% yield) of the pure product. LC-MS found: 214.2.1 (M+H)+.

後処理

temperatureThe reaction mixture was cooled to room temperature
customrecrystallized with methanol

出典と根拠

ORDレコード: ord-67075832b21741ac8627a8bdcca638b1
出典データセット: uspto-grants-2014_11
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08895571B2

反応ノート

読み込み中…

参加物