1,4-Dioxane → HCID 19014324、化合物

HRID 1728549ノート

反応式

HRID 1728549 の反応式
[CH3:1][C:2]1[N:3]=[C:4]([NH:17][CH3:18])[C:5]2[CH:10]=[CH:9][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:6]=2[N:7]=1.O1CCOC[CH2:20]1>>[CH3:1][C:2]1[N:3]([CH3:20])[C:4](=[N:17][CH3:18])[C:5]2[CH:10]=[CH:9][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:6]=2[N:7]=1

参加物

3

反応物 2

HCID 312751,4-DioxaneHCID 19014333N,2-Dimethyl-7-phenyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine

生成物 1

HCID 19014324HCID 19014324、化合物

実験手順

A mixture of 2-methyl-4-methylamino-7-phenyl-7H-pyrrolo-[2,3-d] pyrimidine (0.5g, 2.1mM) and dioxan (15ml) was heated under reflux for 18 hours. The mixture was cooled and then the solvent was removed by evaporation. The residue was purified by flash chromatography on ICN neutral alumina (32-63) using methylene chloride which contained an increasing amount of methanol (up to a maximum of 5%) as eluant to give a solid. This solid was recrystallised from hexane to give 2,3-dimethyl-4-methylimino-7-phenyl-3H,7H-pyrrolo[2,3-d] pyrimidine as a white solid (126mg), m p. 160-161° C; microanalysis, found: C, 71 2; H,5 9; N,22.0%; C14H14N4 requires C,71.4; H, 6.3; N, 22.2%; NMR: 2.48(3H,s,C-CH3), 3.48 (3H,s,N-CH3), 3.56(3H,s,N-CH3), 6.90(1H,d,CH), 6.97(1H,d,CH), 7.34(1H, complex, aromatic), 7.47(2H, complex, aromatic), 7.60(1H, complex, aromatic).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. temperatureThe mixture was cooled
  4. customthe solvent was removed by evaporation
  5. customThe residue was purified by flash chromatography on ICN neutral alumina (32-63)
  6. customto give a solid
  7. customThis solid was recrystallised from hexane

出典と根拠

ORDレコード
ord-9b22da2a913e436a8f35130a03a09de6
出典データセット
uspto-grants-1994_07
特許番号
US05328910

反応ノート

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