1,1,1-Trifluoro-2-isothiocyanatoethane → 4-[3-(2,2,2-Trifluoroethyl)thioureido]-2-(4-phthalimidobutylthio)pyrimidine

HRID 34779

反応式

HRID 34779 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([S:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]2[C:17](=[O:18])[C:16]3=[CH:19][CH:20]=[CH:21][CH:22]=[C:15]3[C:14]2=[O:23])[N:3]=1.[F:24][C:25]([F:31])([F:30])[CH2:26][N:27]=[C:28]=[S:29]>C(#N)C>[F:24][C:25]([F:31])([F:30])[CH2:26][NH:27][C:28](=[S:29])[NH:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([S:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]2[C:14](=[O:23])[C:15]3=[CH:22][CH:21]=[CH:20][CH:19]=[C:16]3[C:17]2=[O:18])[N:3]=1

参加物

4

反応物 2

HCID 138837771,1,1-Trifluoro-2-isothiocyanatoethane2 回HCID 212987544-Amino-2-(4-phthalimidobutylthio)pyrimidine

生成物 1

HCID 542546584-[3-(2,2,2-Trifluoroethyl)thioureido]-2-(4-phthalimidobutylthio)pyrimidine収率 69.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 4-amino-2-(4-phthalimidobutylthio)pyrimidine (0.49 g.), acetonitrile (5 ml.) and 2,2,2-trifluoroethylisothiocyanate (0.28 g.) was stirred at 70° for 48 hours. A further 0.28 g. of 2,2,2-trifluoroethylisothiocyanate was added and the mixture stirred at 70° for 48 hours. The reaction mixture was cooled and filtered, the residue stirred with N aqueous acetic acid and the undissolved solid collected to give 4-[3-(2,2,2-trifluoroethyl)thioureido]-2-(4-phthalimidobutylthio)pyrimidine (0.49 g.), m.p. 201°-202° after recrystallisation from a mixture of ethanol and dimethylformamide.

後処理

  1. stirringthe mixture stirred at 70° for 48 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. stirringthe residue stirred with N aqueous acetic acid
  5. customthe undissolved solid collected

出典と根拠

ORDレコード
ord-d7d0eebacced4eeb9401093813d6f3e1
出典データセット
uspto-grants-1988_08
特許番号
US04762932

関連ノート

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