反応式
[CH2:1]([O:3][C:4]([C:6]1[C:7]2[C:22](=[O:23])[CH:21]=[CH:20][CH2:19][CH2:18][C:8]=2[N:9]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH:10]=1)=[O:5])[CH3:2].[Li+].[F-].[CH2:26]([N:33]([CH2:39]OC)[CH2:34][Si](C)(C)C)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.O>CC#N>[CH2:1]([O:3][C:4]([C:6]1[C:7]2[C:22](=[O:23])[CH:21]3[CH2:34][N:33]([CH2:26][C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[CH2:39][CH:20]3[CH2:19][CH2:18][C:8]=2[N:9]([C:11]([O:13][C:14]([CH3:17])([CH3:15])[CH3:16])=[O:12])[CH:10]=1)=[O:5])[CH3:2]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
4-Oxo-7,8-dihydro-4H-cyclohepta[b]pyrrole-1,3-dicarboxylic acid 1-tert-butyl ester 3-ethyl ester (2.92 g, 9.15 mmol), LiF (296 mg, 11.4 mmol) and benzyl-methoxymethyl-trimethylsilanylmethyl-amine are mixed together in CH3CN (10 ml). The reaction mixture is sonicated under N2. The water bath is kept under 35° C. with ice. After 6 h, solvents are removed in vacuo. The residue is put on a column (1:1 EtOAc hexanes) to afford the title compound as clear oil, which solidified upon standing. 1H NMR (400 MHz, CDCl3) δ 1.23 (3H, t), 1.56 (9H, s), 1.88-2.00 (2H, m), 2.65 (1H, m), 2.92-3.02 (4H, m), 3.24 (1H, m), 3.50-3.59 (3H, m), 4.06 (1H, q), 4.19 (2H, q), 7.18-7.27 (5H, m), 7.62 (1H, s). MS (ES+) 453 (M+1) Step 2: 6-Benzyl4-oxo-4,4a,5,6,7,7a,8,9-octahydro-1H-1,6-diaza-cyclopenta[f]azulene-3-carboxylic acid pyridin-2-ylamide
後処理
- customThe reaction mixture is sonicated under N2
- customis kept under 35° C. with ice
- customsolvents are removed in vacuo
出典と根拠
- ORDレコード
- ord-54f22ada08704b12af2b0d6279320642
- 出典データセット
- uspto-grants-2005_03
- 特許番号
- US06861529B2
関連ノート
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