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

HRID 1698969
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HRID 1698969 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 106795532-Chloro-3-nitrobenzamide

생성물 1

HCID 217860112-Chloro-3-nitrobenzonitrile수율 74%

시약·촉매·용매 1

HCID 131723111P2O5 (TMS)2O 1,2-dichloroethane용매

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온도
25 °C

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-04879d5591c84c1cb31861b2607d6a1f
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06344459B1

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