Morpholine → 4-Morpholino-2-nitrobenzonitrile

HRID 1431289ノート

反応式

HRID 1431289 の反応式
Cl[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.[NH:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1>CS(C)=O>[O:16]1[CH2:17][CH2:18][N:13]([C:2]2[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=2)[CH2:14][CH2:15]1

参加物

4

反応物 2

HCID 8083MorpholineHCID 969244-Chloro-2-nitrobenzonitrile

生成物 1

HCID 134992654-Morpholino-2-nitrobenzonitrile

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of 4-chloro-2-nitrobenzonitrile (7.828 g, 42.9 mmol) and morpholine (4.49 mL, 51.5 mmol) in DMSO (20.00 mL) was stirred at rt for 1 h, after which time LC-MS indicated a small amount of desired product formed. The reaction was heated to 100° C. After 24 h the reaction was equilibrated to rt and poured into 50 mL ea 1N aq. hydrochloric acid and EtOAc. The resulting orange precipitate was collected by filtration, rinsing with EtOAc, then dried under vacuum. Mass Spectrum (ESI) m/e=234.1 (M+1).

出典と根拠

ORDレコード
ord-e1e7caa7668d43da8f0fc115ec48bf8e
出典データセット
uspto-grants-2015_01
特許番号
US08940724B2

反応ノート

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