Methanol → 1-(2-[4-(2-[2,2,2-Trifluoroethyl]guanidino)pyrimid-2-yl-methylthio]ethylamino)-2-methylaminocyclobutene-3,4-dione

HRID 34795

反応式

HRID 34795 の反応式
[F:1][C:2]([F:20])([F:19])[CH2:3][N:4]=[C:5]([NH2:18])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([CH2:13][S:14][CH2:15][CH2:16][NH2:17])[N:8]=1.CO.C[O:24][C:25]1[C:28](=O)[C:27](=O)[C:26]=1[O:31]C.[CH3:33][NH2:34]>C(O)C>[F:20][C:2]([F:1])([F:19])[CH2:3][N:4]=[C:5]([NH2:18])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([CH2:13][S:14][CH2:15][CH2:16][NH:17][C:28]2[C:25](=[O:24])[C:26](=[O:31])[C:27]=2[NH:34][CH3:33])[N:8]=1

参加物

6

反応物 4

HCID 887MethanolHCID 6329MethylamineHCID 1232273-Cyclobutene-1,2-dione, 3,4-dimethoxy-HCID 212987204-[2-(2,2,2-Trifluoroethyl)guanidino]-2-(2-aminoethyl)thiomethylpyrimidine

生成物 1

HCID 212988481-(2-[4-(2-[2,2,2-Trifluoroethyl]guanidino)pyrimid-2-yl-methylthio]ethylamino)-2-methylaminocyclobutene-3,4-dione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-(2-aminoethyl)thiomethylpyrimidine (0.31 g.), methanol (5 ml.) and 1,2-dimethoxycyclobutene-3,4-dione (0.14 g.) was stirred at room temperature for 18 hours. A 33% w/v solution of methylamine in ethanol (5 ml.) was added and the mixture left at room temperature for 18 hours and then evaporated to dryness. The residue was purified by preparative thin layer chromatography using ethyl acetate/methanol/ammonia 6:1:0.5 v/v/v as developing solvent to give 1-(2-[4-(2-[2,2,2-trifluoroethyl]guanidino)pyrimid-2-yl-methylthio]ethylamino)-2-methylamino cyclobutene-3,4-dione (0.16 g.) characterised as the hydrogen maleate, m.p. 178°-184° after recrystallisation from a mixture of methanol and acetonitrile.

後処理

  1. additionwas added
  2. waitthe mixture left at room temperature for 18 hours
  3. customevaporated to dryness
  4. customThe residue was purified by preparative thin layer chromatography

出典と根拠

ORDレコード
ord-26e078658ecd425db22abce78d4b93a2
出典データセット
uspto-grants-1988_08
特許番号
US04762932

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