Ethanol → HCID 86742227、化合物

反応式

[Cl-].[NH4+:2].[OH-].[NH4+].[CH3:5][O:6][N:7]=[C:8]([C:11]#[N:12])[C:9]#[N:10].[CH2:13]([OH:15])[CH3:14]>>[C:13]([O-:6])(=[O:15])[CH3:14].[C:9]([C:8](=[N:7][O:6][CH3:5])[C:11]([NH2:2])=[NH2+:12])#[N:10]

参加物

反応物 4

HCID 702Ethanol

HCID 14923Ammonium Hydroxide

HCID 25517Ammonium Chloride

HCID 12474891Methoxyiminomalononitrile

生成物 1

HCID 86742227HCID 86742227、化合物

実験手順

To a mixed solution of ammonium chloride(14.2 g) dissolved in ethanol (90 ml) and conc. ammonium hydroxide aqueous solution (178 ml) was added 2-(methoxyimino)malononitrile(29 g) at -5°~0° C., and the mixture was stirred for 10 hours at these temperatures. The reaction mixture was extracted 3 times with methylene chloride (respectively, 450 ml, 100 ml and 100 ml), dehydrated, filtered, and concentrated. The residue was dissolved in ethyl acetate, and crystalized with acetic acid to give the above-indicated compound (20.5 g) in pale brown.

後処理

extractionThe reaction mixture was extracted 3 times with methylene chloride (respectively, 450 ml, 100 ml and 100 ml),
filtrationfiltered
concentrationconcentrated
dissolutionThe residue was dissolved in ethyl acetate
customcrystalized with acetic acid

出典と根拠

ORDレコード: ord-71cffb89e4f34f9d82b9a41ba55ce076
出典データセット: uspto-grants-1993_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05202315

反応ノート

読み込み中…

参加物