反応式
[CH3:1][O:2][C:3](=[O:15])[CH2:4][CH2:5][NH:6][CH2:7][C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].[NH:16]([C:46]([O:48][CH2:49][C:50]1[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1)=[O:47])[C@H:17]([C:43](O)=[O:44])[CH2:18][C:19]1[N:23]=[CH:22][N:21]([C:24]([C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:20]=1.C(N(CC)CC)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>C(Cl)Cl.C(#N)C>[CH3:1][O:2][C:3](=[O:15])[CH2:4][CH2:5][N:6]([C:43](=[O:44])[C@@H:17]([NH:16][C:46]([O:48][CH2:49][C:50]1[CH:51]=[CH:52][CH:53]=[CH:54][CH:55]=1)=[O:47])[CH2:18][C:19]1[N:23]=[CH:22][N:21]([C:24]([C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:20]=1)[CH2:7][C:8]([O:10][C:11]([CH3:12])([CH3:14])[CH3:13])=[O:9]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
To a solution of the compound from Step 1 (0.434 g, 2 mmol) in methylene chloride (10 mL) was added Cbz-His(Trt)-OH (1.062 g, 2 mmol), triethylamine (0.8 mL, 5.7 mmol) and HBTU (0.758 g, 2 mmol) dissolved in acetonitrile (10 mL). The reaction mixture was stirred overnight at room temperature. The solution was concentrated, the residue taken up in ethyl acetate and washed three times with saturated NaHCO3, brine, dried over MgSO4, filtered and concentrated in vacuo. Chromatography was carried out on silica gel, using 30% hexanes in ethyl acetate as eluent, to give an oil; 1.38 g (94% yield). MS-APCI: M+1=732.
後処理
- concentrationThe solution was concentrated
- washwashed three times with saturated NaHCO3, brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give an oil
出典と根拠
- ORDレコード
- ord-7b8cf208f08d49fab90c7b5c1af1990d
- 出典データセット
- uspto-grants-2002_04
- 特許番号
- US06369034B1
関連ノート
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