N-Iodosuccinimide → HCID 67494276, 화합물

HRID 2047008노트

반응식

HRID 2047008 반응식
[I:1]N1C(=O)CCC1=O.[CH3:9][Si:10]([CH3:54])([CH3:53])[CH2:11][CH2:12][O:13][CH2:14][N:15]([CH2:45][O:46][CH2:47][CH2:48][Si:49]([CH3:52])([CH3:51])[CH3:50])[C:16]1[N:21]2[N:22]=[CH:23][CH:24]=[C:20]2[N:19]=[C:18]([CH:25]2[CH2:30][N:29]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH:28]([C:38]([O:40][C:41]([CH3:44])([CH3:43])[CH3:42])=[O:39])[CH2:27][CH2:26]2)[CH:17]=1>C(#N)C>[CH3:52][Si:49]([CH3:50])([CH3:51])[CH2:48][CH2:47][O:46][CH2:45][N:15]([CH2:14][O:13][CH2:12][CH2:11][Si:10]([CH3:9])([CH3:53])[CH3:54])[C:16]1[N:21]2[N:22]=[CH:23][C:24]([I:1])=[C:20]2[N:19]=[C:18]([CH:25]2[CH2:30][N:29]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH:28]([C:38]([O:40][C:41]([CH3:43])([CH3:44])[CH3:42])=[O:39])[CH2:27][CH2:26]2)[CH:17]=1

참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 67494273HCID 67494273, 화합물

생성물 1

HCID 67494276HCID 67494276, 화합물수율 70.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

N-Iodosuccinimide (1.26 g, 5.61 mmol, dissolved in 25 ml acetonitrile) was added into a solution of di-tert-butyl 5-(7-(bis((2-(trimethylsilyl)ethoxy)methyl)amino)pyrazolo[1,5-a]pyrimidin-5-yl)piperidine-1,2-dicarboxylate (3.8 g, 5.61 mmol) in acetonitrile (26 mL). The reaction mixture was stirred at room temperature for 16 hours. The reaction mixture was concentrated in vacuo and purified via silica gel chromatography (0% to 30% ethyl acetate in hexanes gradient) to yield the title compound (3.16 g, 70% yield) at clear oil. LC-MS: 804 [M+H].

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. custompurified via silica gel chromatography (0% to 30% ethyl acetate in hexanes gradient)

출처 및 근거

ORD 기록
ord-3b2c1edd314f46f7b29a3489603edffc
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08591943B2

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