반응식
CC[N:3]([CH:7]([CH3:9])C)[CH:4](C)C.[OH:10][CH2:11][C@H:12]([CH3:40])[O:13][C:14]1[CH:15]=[C:16]([CH:27]=[C:28]([C:30]([NH:32][C:33]2[CH:38]=[N:37][C:36]([CH3:39])=[CH:35][N:34]=2)=[O:31])[CH:29]=1)[O:17][C:18]1[CH:26]=[CH:25][C:21]([C:22](O)=[O:23])=[CH:20][CH:19]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl.N1CCC1>CN(C=O)C.O>[N:3]1([C:22]([C:21]2[CH:20]=[CH:19][C:18]([O:17][C:16]3[CH:27]=[C:28]([CH:29]=[C:14]([O:13][C@@H:12]([CH3:40])[CH2:11][OH:10])[CH:15]=3)[C:30]([NH:32][C:33]3[CH:38]=[N:37][C:36]([CH3:39])=[CH:35][N:34]=3)=[O:31])=[CH:26][CH:25]=2)=[O:23])[CH2:4][CH2:9][CH2:7]1참가 물질
7
반응물 4
HCID 81531Diisopropylethylamine
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 12308726Azetidine hydrochloride
HCID 593469134-(3-[(1S)-2-hydroxy-1-methylethoxy]-5-{[(5-methylpyrazin-2-yl)amino]carbonyl}phenoxy)benzoic acid생성물 1
시약·촉매·용매 2
실험 절차
DIPEA (0.4 mL, 2.08 mmol) was added to a suspension of 4-(3-[(1S)-2-hydroxy-1-methylethoxy]-5-{[(5-methylpyrazin-2-yl)amino]carbonyl}phenoxy)benzoic acid (110 mg, 0.26 mmol), HATU (210 mg, 0.55 mmol) and azetidine hydrochloride (49 mg, 0.52 mmol) in DMF (3 mL) and the mixture stirred at RT for 24 hours. Water (30 mL) was added and the mixture extracted with ethyl acetate (3×15 mL). The combined organic extracts were washed with brine, dried (MgSO4), and evaporated to a residue which was chromatographed on silica, eluting with 5% methanol in ethyl acetate, to give the desired compound (55 mg).
후처리
- extractionthe mixture extracted with ethyl acetate (3×15 mL)
- washThe combined organic extracts were washed with brine
- dry with materialdried (MgSO4)
- customevaporated to a residue which
- customwas chromatographed on silica
- washeluting with 5% methanol in ethyl acetate
출처 및 근거
- ORD 기록
- ord-ce28fb4cf5104a12903315a39263e4f3
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07745475B2
연결된 노트
불러오는 중…