反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[NH:9][S:10]([C:13]1[CH:14]=[C:15]([CH:19]=[CH:20][CH:21]=1)[C:16]([OH:18])=O)(=[O:12])=[O:11].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH2:46]1[NH:51][CH2:50][CH2:49][N:48]2[CH2:52][CH2:53][CH2:54][C@H:47]12>CN(C)C(=O)C.CC1CCCO1>[F:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[C:3]=1[NH:9][S:10]([C:13]1[CH:21]=[CH:20][CH:19]=[C:15]([C:16]([N:51]2[CH2:50][CH2:49][N:48]3[CH2:52][CH2:53][CH2:54][C@@H:47]3[CH2:46]2)=[O:18])[CH:14]=1)(=[O:12])=[O:11]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
To 3-{[(2,6-difluorophenyl)amino]sulfonyl}benzoic acid (0.96 g, 3.06 mmol) and 2-(3H-[1,2,3]triazolo[4,5-b]pyridin-3-yl)-1,1,3,3-tetramethylisouronium hexafluorophosphate(V) (1.28 g, 3.37 mmol) in N,N-dimethylacetamide (7.4 mL) and 2-methyltetrahydrofuran (22 mL) was added (R)-octahydropyrrolo[1,2-a]pyrazine (0.54 g, 4.28 mmol). The reaction was stirred at ambient temperature for 5.5 hours, and then it was diluted with 2-methyltetrahydrofuran (15 mL). The organic solution was washed with 6% NaHCO3/6% NaCl (35 mL), and the aqueous layer was extracted with 2-methyltetrahydrofuran (50 mL). The organic layer was washed with 6% NaHCO3/6% NaCl (50 mL) and 1:1 saturated NaCl/water (6×15 mL), and then it was concentrated. The residue was concentrated from ethanol (2×10 mL) to give the title compound.
後処理
- washThe organic solution was washed with 6% NaHCO3/6% NaCl (35 mL)
- extractionthe aqueous layer was extracted with 2-methyltetrahydrofuran (50 mL)
- washThe organic layer was washed with 6% NaHCO3/6% NaCl (50 mL) and 1:1 saturated NaCl/water (6×15 mL)
- concentrationit was concentrated
- concentrationThe residue was concentrated from ethanol (2×10 mL)
出典と根拠
- ORDレコード
- ord-69a6d0901ad14203a310d400d590708b
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08741899B2
関連ノート
読み込み中…