3-((Tert-butyldiphenylsilyl)oxy)azetidine → HCID 54591371, 화합물

HRID 1260189노트

반응식

HRID 1260189 반응식
Br[C:2]1[CH:3]=[C:4]([CH:30]=[CH:31][CH:32]=1)[CH2:5][N:6]1[C:10]([CH3:11])=[CH:9][C:8]([C:12]2[O:16][N:15]=[C:14]([C:17]3[CH:22]=[CH:21][C:20]([C:23]([CH3:29])([CH3:28])[C:24]([F:27])([F:26])[F:25])=[CH:19][CH:18]=3)[N:13]=2)=[N:7]1.[Si]([O:50][CH:51]1[CH2:54][NH:53][CH2:52]1)(C(C)(C)C)(C1C=CC=CC=1)C1C=CC=CC=1>>[CH3:11][C:10]1[N:6]([CH2:5][C:4]2[CH:3]=[C:2]([N:53]3[CH2:54][CH:51]([OH:50])[CH2:52]3)[CH:32]=[CH:31][CH:30]=2)[N:7]=[C:8]([C:12]2[O:16][N:15]=[C:14]([C:17]3[CH:22]=[CH:21][C:20]([C:23]([CH3:29])([CH3:28])[C:24]([F:27])([F:26])[F:25])=[CH:19][CH:18]=3)[N:13]=2)[CH:9]=1

참가 물질

3

반응물 2

HCID 178425313-((Tert-butyldiphenylsilyl)oxy)azetidineHCID 58072152HCID 58072152, 화합물

생성물 1

HCID 54591371HCID 54591371, 화합물

실험 절차

Analogously to the process described in Example 1, 150 mg (0.297 mmol) of the compound from Example 3A and 139 mg (0.445 mmol) of the compound from Example 8A were used to obtain 68 mg (46% of theory) of the title compound. The reaction time in the first component step of the process here was 1 h. The crude product was purified by means of preparative HPLC (method 13). The free base was obtained from the resulting formate salt of the title compound by percolation of a methanolic solution of the salt through a hydrogencarbonate cartridge (from Polymerlabs, Stratospheres SPE, PL-HCO3 MP SPE, capacity 0.9 mmol). The final purification was effected by extractive stirring in a mixture of 3 ml of pentane and a few drops of diisopropyl ether.

출처 및 근거

ORD 기록
ord-ad556528ce54479698da0205873fefa2
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08470811B2

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