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

HRID 2069197ノート

反応式

HRID 2069197 の反応式
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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-7eea605b2502417b98ad5e2a74b1f462
出典データセット
uspto-grants-2012_10
特許番号
US08299085B2

反応ノート

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