반응식
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:13]=[C:12]2[C:8]([CH2:9][CH2:10][CH2:11]2)=[CH:7][C:6]=1[NH:14][S:15]([C:18]1[S:19][CH:20]=[C:21]([CH3:23])[N:22]=1)(=[O:17])=[O:16].C(P(CCCC)CCCC)CCC.[F:37][C@@H:38]([CH3:41])[CH2:39]O.N(/C(N1CCCCC1)=O)=N\C(N1CCCCC1)=O>C1COCC1>[F:37][C@@H:38]([CH3:41])[CH2:39][N:14]([C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][C:5]=1[O:4][CH2:3][O:2][CH3:1])[CH2:11][CH2:10][CH2:9]2)[S:15]([C:18]1[S:19][CH:20]=[C:21]([CH3:23])[N:22]=1)(=[O:17])=[O:16]참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
896 mg of N-[6-(methoxymethoxy)-2,3-dihydro-1H-inden-5-yl]-4-methyl-1,3-thiazole-2-sulfonamide, 665 mg of tributyl phosphine, and 257 mg of (2S)-2-fluoropropan-1-ol were dissolved in 8.96 mL of THF, and 829 mg of 1,1′-[(E)-diazen-1,2-diyldicarbonyl]dipiperidine was added thereto, followed by stirring overnight at room temperature. After the insoluble materials were removed by filtration, the filtrate was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:10 to 50:50) to obtain 632 mg of N-[(2S)-2-fluoropropyl]-N-[6-(methoxymethoxy)-2,3-dihydro-1H-inden-5-yl]-4-methyl-1,3-thiazole-2-sulfonamide.
후처리
- customAfter the insoluble materials were removed by filtration
- concentrationthe filtrate was concentrated under reduced pressure
- customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:10 to 50:50)
출처 및 근거
- ORD 기록
- ord-35ad8660e8664d61bd5bd05f70e8665a
- 출처 데이터셋
- uspto-grants-2012_11
- 특허 번호
- US08314240B2
연결된 노트
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