Pyridine → Methyl 2,6-dichloro-4-cyanobenzoate

反応式

[C:1]([C:4]1[CH:13]=[C:12]([Cl:14])[C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:6]([Cl:15])[CH:5]=1)(=O)[NH2:2].N1C=CC=CC=1>>[Cl:14][C:12]1[CH:13]=[C:4]([C:1]#[N:2])[CH:5]=[C:6]([Cl:15])[C:7]=1[C:8]([O:10][CH3:11])=[O:9]

参加物

反応物 2

HCID 1049Pyridine

HCID 67128947Methyl 4-carbamoyl-2,6-dichlorobenzoate

生成物 1

HCID 53401291Methyl 2,6-dichloro-4-cyanobenzoate収率 88%

実験手順

To a solution of methyl 4-carbamoyl-2,6-dichlorobenzoate (100 mg, 0.4 mmol) in pyridine (2 mL) trifluoro-acetic anhydride (0.11 ml, 0.8 mmol) was added drop wise at 0° C. The reaction mixture was allowed to warm to room temperature and stirred for 1 hour. The contents were poured into ice cold water and the precipitated solid was filtered, washed with water and dried to yield methyl 2,6-dichloro-4-cyanobenzoate (55 mg, 88%) as an off-white solid.

後処理

additionThe contents were poured into ice cold water
filtrationthe precipitated solid was filtered
washwashed with water
customdried

出典と根拠

ORDレコード: ord-cdc5d0a09c8440c083679e1d0224347f
出典データセット: uspto-grants-2016_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09364466B2

反応ノート

読み込み中…

参加物