Potassium thiocyanate → (2-Bromo-4,6-dinitro-phenyl) thiocyanate
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[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]=1Br.[S-:15][C:16]#[N:17].[K+]>CO>[Br:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]=1[S:15][C:16]#[N:17]참가 물질
4
실험 절차
To a stirred solution of 1,2-dibromo-3,5-dinitrobenzene (723 g, 2.22 mol) in MeOH (7.5 L) at rt was added potassium thiocyanate (431 g, 4.44 mol) and the resulting reaction mixture stirred under a nitrogen atmosphere for 16 h. The reaction mixture was then filtered and washed with methanol. The filtrate was concentrated at 30-33° C. under reduced pressure. The residue thus obtained was purified over silica gel (2-6% EtOAc-hexane) to obtain the desired product (549 g, 81%).
후처리
- customthe resulting reaction mixture
- filtrationThe reaction mixture was then filtered
- washwashed with methanol
- concentrationThe filtrate was concentrated at 30-33° C. under reduced pressure
- customThe residue thus obtained
- customwas purified over silica gel (2-6% EtOAc-hexane)
출처 및 근거
- ORD 기록
- ord-b25ab365dbe545558558fe4e0fff602f
- 출처 데이터셋
- uspto-grants-2015_11
- 특허 번호
- US09181234B2
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