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Acetic Anhydride → HCID 178474345, 화합물

HRID 537024
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HRID 537024 반응식
COC1C=C(OC)C=C[C:4]=1[CH2:5][NH:6][C:7]1[N+:8]([O-:17])=[CH:9][C:10]([CH3:16])=[C:11]([N+:13]([O-:15])=[O:14])[CH:12]=1.C(OC(=O)C)(=[O:26])C>C(Cl)Cl.C(O)(C(F)(F)F)=O>[CH3:16][C:10]1[C:11]([N+:13]([O-:15])=[O:14])=[CH:12][C:7]([NH:6][C:5](=[O:26])[CH3:4])=[N+:8]([O-:17])[CH:9]=1
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참가 물질

5

반응물 2

HCID 7918Acetic AnhydrideHCID 178490961HCID 178490961, 화합물

생성물 1

HCID 178474345HCID 178474345, 화합물수율 98.8%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of N-(2,4-dimethoxybenzyl)-5-methyl-4-nitropyridin-2-amine 1-oxide (1.1 g, 3.5 mmol) in DCM (20 mL) and TFA (3 mL) was allowed to stir at rt for 4 h. The reaction mixture was concentrated and the residue was dissolved in DCM (20 mL). To this solution were added TEA (2.5 mL, 17.7 mmol) and acetic anhydride (0.4 g, 4.3 mmol). The reaction mixture was allowed to stir at rt overnight and then filtered to give N-(5-methyl-4-nitro-1-oxidopyridin-2-yl)acetamide (0.73 g, 98%) which was used without further purification.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in DCM (20 mL)
  3. stirringto stir at rt overnight
  4. filtrationfiltered

출처 및 근거

ORD 기록
ord-fe68412fa4544edd807c53fc572c95bb
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859768B2

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