2-Chloro-3-nitrobenzamide → 2-Chloro-3-nitrobenzonitrile

反応式

[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=O>O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.O([Si](C)(C)C)[Si](C)(C)C.ClCCCl>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]#[N:6]

参加物

反応条件

温度: 25 °C

実験手順

A solution of 2-chloro-3-nitrobenzamide (1.02 g, 4.9 mmol) in P2O5/(TMS)2O/1,2-dichloroethane (30 mL) was heated at 85° C. for 18 hours. After it was cooled to 25° C., the solution was filtered through a plug of silica gel (60 mL), eluting with 5% methanol/CHCl3 (400 mL). The combined washes were concentrated under reduced pressure to give 2-chloro-3-nitrobenzonitrile as an off-white solid (0.66 g, 74%).

後処理

filtrationthe solution was filtered through a plug of silica gel (60 mL)
washeluting with 5% methanol/CHCl3 (400 mL)
concentrationThe combined washes were concentrated under reduced pressure

出典と根拠

ORDレコード: ord-6c8414320fed4b1b9a587697551947a5
出典データセット: uspto-grants-2003_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06602863B1

反応ノート

読み込み中…

参加物

反応物 1

HCID 106795532-Chloro-3-nitrobenzamide

生成物 1

HCID 217860112-Chloro-3-nitrobenzonitrile収率 74%

試薬・触媒・溶媒 1

HCID 131723111P2O5 (TMS)2O 1,2-dichloroethane溶媒

反応条件

温度: 25 °C

実験手順

後処理

filtrationthe solution was filtered through a plug of silica gel (60 mL)
washeluting with 5% methanol/CHCl3 (400 mL)
concentrationThe combined washes were concentrated under reduced pressure

出典と根拠

ORDレコード: ord-6c8414320fed4b1b9a587697551947a5
出典データセット: uspto-grants-2003_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06602863B1

反応ノート

読み込み中…