Dimethylformamide → HCID 178485208、化合物

HRID 364281

反応式

HRID 364281 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][NH:14][C:15]([NH:21][CH3:22])=[N:16][S:17]([CH3:20])(=[O:19])=[O:18])[N:3]=1.[F:23][C:24]([F:30])([F:29])[CH2:25][N:26]=[C:27]=S.C[N:32](C)C=O>>[NH2:8][C:6]1[N:7]=[C:2]([NH:1][C:27]([NH2:32])=[N:26][CH2:25][C:24]([F:30])([F:29])[F:23])[N:3]=[C:4]([CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][NH:14][C:15]([NH:21][CH3:22])=[N:16][S:17]([CH3:20])(=[O:19])=[O:18])[N:5]=1

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 138837771,1,1-Trifluoro-2-isothiocyanatoethaneHCID 178485209HCID 178485209、化合物

生成物 1

HCID 178485208HCID 178485208、化合物

実験手順

A mixture of 2,4-diamino-6-[5-(2-methanesulphonyl-3-methylguanidino)pentyl]-1,3,5-triazine (0.4 g.), 2,2,2-trifluoroethylisothiocyanate (0.4 g.) and dimethylformamide (0.5 ml.) was heated at 120° for 1 hour and then at 60° for 18 hours. The mixture was evaporated to dryness, the residue partitioned between water and ethyl acetate, and the ethyl phase was separated, dried, and evaporated to dryness. The residue was dissolved in saturated ethanolic ammonia (10 ml.) and the solution treated with yellow mercuric oxide (0.5 g.). The mixture was stirred at room temperature for 18 hours, filtered and the filtrate evaporated to dryness. The residue was purified by chromatography using ethyl acetate/methanol/ammonia 6:1:0.5 v/v/v as developing solvent to give 2-amino-4-[2-(2,2,2-trifluoroethyl)guanidino]-6-[5-(2-methanesulphonyl-3-methylguanidino)pentyl]-1,3,5-triazine (0.07 g.) characterised as the bishydrogen maleate, m.p. 131°-133° after recrystallisation from acetone.

後処理

  1. temperaturewas heated at 120° for 1 hour
  2. customThe mixture was evaporated to dryness
  3. customthe residue partitioned between water and ethyl acetate
  4. customthe ethyl phase was separated
  5. customdried
  6. customevaporated to dryness
  7. dissolutionThe residue was dissolved in saturated ethanolic ammonia (10 ml.)
  8. additionthe solution treated with yellow mercuric oxide (0.5 g.)
  9. filtrationfiltered
  10. customthe filtrate evaporated to dryness
  11. customThe residue was purified by chromatography

出典と根拠

ORDレコード
ord-cbb8e32765b148da8178a6068fd1ba9d
出典データセット
uspto-grants-1986_08
特許番号
US04604465

関連ノート

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