Dimethylformamide → HCID 178485208, 화합물

HRID 364281

반응식

HRID 364281 반응식
[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

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 138837771,1,1-Trifluoro-2-isothiocyanatoethaneHCID 178485209HCID 178485209, 화합물

생성물 1

HCID 178485208HCID 178485208, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cbb8e32765b148da8178a6068fd1ba9d
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04604465

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