반응식
[CH3:1][O:2][C:3]([C:5]1[N:6]([NH:10][C:11](=[O:21])[CH2:12][O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:7]=[N:8][CH:9]=1)=[O:4].[CH2:22](OC(C)C(O)=O)C1C=CC=CC=1.CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C1COCC1.O>[CH3:1][O:2][C:3]([C:5]1[N:6]([NH:10][C:11](=[O:21])[CH:12]([O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH3:22])[CH:7]=[N:8][CH:9]=1)=[O:4]참가 물질
8
반응물 4
생성물 1
시약·촉매·용매 3
실험 절차
To a solution of compound 2 (4.2 g, 29.7 mmol), 2-Benzyloxy-propionic acid (5.5 g, 29.7 mmol) and DIEA (10 mL) in a mixture of DMF (1 mL) and THF (50 mL) in ice-water bath was added HATU (13.5 g, 35.7 mmol). The resulting mixture was then stirred at ambient temperature overnight. Water (100 mL) was added. The mixture was extracted with ethyl acetate (300 mL×2). The combined organic phases were concentrated to give a crude residue, which was purified by chromatography on silica gel column (eluted with PE/EtOAc=1:1 to 1:3) to afford compound 9 (8.2 g, 91% yield) as brown oil. LC-MS: m/z 304 [M+H]+.
후처리
- extractionThe mixture was extracted with ethyl acetate (300 mL×2)
- concentrationThe combined organic phases were concentrated
- customto give a crude residue, which
- customwas purified by chromatography on silica gel column (eluted with PE/EtOAc=1:1 to 1:3)
출처 및 근거
- ORD 기록
- ord-efc87d032fbe4100bf345dd07e40e300
- 출처 데이터셋
- uspto-grants-2016_09
- 특허 번호
- US09434733B2
연결된 노트
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