N-Iodosuccinimide → HCID 67494276、化合物

HRID 2047008ノート

反応式

HRID 2047008 の反応式
[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

参加物

4

反応物 2

HCID 120273N-IodosuccinimideHCID 67494273HCID 67494273、化合物

生成物 1

HCID 67494276HCID 67494276、化合物収率 70.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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].

後処理

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

出典と根拠

ORDレコード
ord-3b2c1edd314f46f7b29a3489603edffc
出典データセット
uspto-grants-2013_11
特許番号
US08591943B2

反応ノート

読み込み中…