Hydrochloric Acid → Anthranilic acid, N,N-bis(2-chloroethyl)-

反応式

[Cl:1][CH2:2][CH2:3][N:4]([C:8]1[CH:18]=[CH:17][CH:16]=[CH:15][C:9]=1[C:10]([O:12]CC)=[O:11])[CH2:5][CH2:6][Cl:7].Cl>>[Cl:1][CH2:2][CH2:3][N:4]([C:8]1[CH:18]=[CH:17][CH:16]=[CH:15][C:9]=1[C:10]([OH:12])=[O:11])[CH2:5][CH2:6][Cl:7]

参加物

反応物 2

HCID 313Hydrochloric Acid

HCID 22096864HCID 22096864、化合物

生成物 1

HCID 18333Anthranilic acid, N,N-bis(2-chloroethyl)-収率 61%

実験手順

Ethyl 2-[N,N-bis(2-chloroethyl)amino]benzoate (950 mg; 3.3 mmol) was added to 15 ml of concentrated hydrochloric acid, followed by stirring for 8 hours under heating and reflux. The solvent was distilled out under reduced pressure and the residue was purified by chromatography on a silica gel column (methylene chloride→acetone), whereby 520 mg of white powder were obtained (yield: 61%).

後処理

temperatureunder heating
temperaturereflux
distillationThe solvent was distilled out under reduced pressure
customthe residue was purified by chromatography on a silica gel column (methylene chloride→acetone)

出典と根拠

ORDレコード: ord-9def897171234c70a776828ed13295e9
出典データセット: uspto-grants-1998_12
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05852011

反応ノート

読み込み中…

参加物