Trifluoroacetic acid → N-(6-Amino-7-nitro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide

HRID 2069197노트

반응식

HRID 2069197 반응식
COC1C=C(OC)C=CC=1C[NH:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[N+:17]([O-:19])=[O:18])[NH:13][C:12](=[O:20])[N:11]([NH:21][S:22]([CH3:25])(=[O:24])=[O:23])[C:10]2=[O:26].FC(F)(F)C(O)=O>ClCCl.C(OCC)C>[NH2:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[N+:17]([O-:19])=[O:18])[NH:13][C:12](=[O:20])[N:11]([NH:21][S:22]([CH3:25])(=[O:23])=[O:24])[C:10]2=[O:26]

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acidHCID 58964506N-[6-(2,4-dimethoxy-benzylamino)-7-nitro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl]-methanesulfonamide

생성물 1

HCID 11674068N-(6-Amino-7-nitro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

To a solution of N-[6-(2,4-dimethoxy-benzylamino)-7-nitro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl]-methanesulfonamide (725 mg, 1.56 mmol) in dichloromethane (4 ml) is added trifluoroacetic acid (0.5 ml) and the mixture is stirred at room temperature for 30 minutes. Then the solvent is removed by rotavapor evaporation to give an orange solid which is suspended in diethyl ether, filtered and the residue washed 3 times with diethyl ether and two times with ethyl acetate to give the title product as a pure orange solid, m.p. 326-335° C. (decomp.).

후처리

  1. customThen the solvent is removed by rotavapor evaporation
  2. customto give an orange solid which
  3. filtrationfiltered
  4. washthe residue washed 3 times with diethyl ether and two times with ethyl acetate

출처 및 근거

ORD 기록
ord-7eea605b2502417b98ad5e2a74b1f462
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299085B2

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