반응식
[F:1][C:2]([F:23])([F:22])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][S:10]([C:13]2[CH:14]=[C:15]([CH:19]=[CH:20][CH:21]=2)[C:16](O)=[O:17])(=[O:12])=[O:11])=[CH:5][CH:4]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[N:48]12[CH2:57][CH2:56][CH2:55][CH2:54][CH:53]1[CH2:52][NH:51][CH2:50][CH2:49]2>CN(C)C(=O)C.CC1CCCO1>[CH2:52]1[N:51]([C:16]([C:15]2[CH:14]=[C:13]([S:10]([NH:9][C:6]3[CH:7]=[CH:8][C:3]([C:2]([F:22])([F:23])[F:1])=[CH:4][CH:5]=3)(=[O:11])=[O:12])[CH:21]=[CH:20][CH:19]=2)=[O:17])[CH2:50][CH2:49][N:48]2[CH2:57][CH2:56][CH2:55][CH2:54][CH:53]12참가 물질
반응물 3
생성물 1
시약·촉매·용매 2
실험 절차
To 3-({[4-(trifluoromethyl)phenyl]amino}sulfonyl)benzoic acid (4.35 g, 12.6 mmol) and 2-(3H-[1,2,3]triazolo[4,5-b]pyridin-3-yl)-1,1,3,3-tetramethylisouronium hexafluorophosphate(V) (5.27 g, 13.9 mmol) in N,N-dimethylacetamide (30 mL) and 2-methyltetrahydrofuran (90 mL) was added 1,4-diazabicyclo[4.4.0]decane (2.47 g, 17.6 mmol). The reaction was stirred at ambient temperature for 2.5 hours, and then it was diluted with 2-methyltetrahydrofuran (57 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 (6×50 mL), and then it was concentrated. The residue was concentrated from ethanol (2×50 mL) to give the title compound.
후처리
- 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 (6×50 mL)
- concentrationit was concentrated
- concentrationThe residue was concentrated from ethanol (2×50 mL)
출처 및 근거
- ORD 기록
- ord-5f29be97ee954137801b2172c6d53de7
- 출처 데이터셋
- uspto-grants-2014_06
- 특허 번호
- US08741899B2
연결된 노트
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