Trifluoroacetic acid → 5H,6H,7H,8H-pyrido(4,3-d)pyrimidine
反応式
C(OC([N:8]1[CH2:17][CH2:16][C:11]2[N:12]=[CH:13][N:14]=[CH:15][C:10]=2[CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[N:12]1[C:11]2[CH2:16][CH2:17][NH:8][CH2:9][C:10]=2[CH:15]=[N:14][CH:13]=1参加物
4
実験手順
A solution of the product from Step B above (730 mg) in 10 mL of dichloromethane was cooled to 0° C. and treated dropwise with 5 mL of trifluoroacetic acid. The solution was warmed to room temperature and, after 1 h, concentrated under reduced pressure. The residue was dissolved in methanol and applied to an ion-exchange column (Varian Bond-Elut SCX, 5 g; preconditioned with methanol). The column was washed several times with methanol, and the amine product was eluted with 1.0M ammonia-methanol. The fractions containing product were concentrated under reduced pressure to afford the title compound as an orange oil. LC/MS 136.1 (M+1).
後処理
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in methanol
- washThe column was washed several times with methanol
- washthe amine product was eluted with 1.0M ammonia-methanol
- additionThe fractions containing product
- concentrationwere concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-ef19a511793b467d831426803023479c
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653059B2
反応ノート
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