反応式
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=O)=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C.[NH:36]1[CH2:41][CH2:40][O:39][CH2:38][CH2:37]1>CN(C=O)C.O.C(N(CC)CC)C>[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([N:36]2[CH2:41][CH2:40][O:39][CH2:38][CH2:37]2)=[O:8])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 3
実験手順
The compound ([5]-(53)-278) (6.5272 g) prepared in Example 72 was dissolved in anhydrous DMF (98 ml). Then, 1-hydroxybenzotriazole (6.3297 g), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (8.9795 g), triethylamine (6.5 ml), and morpholine (4.1 ml) were added to the solution. The mixture was stirred at room temperature for 4 hours. A small amount of water was added to the resulting yellowish orange solution including the white salt to obtain a homogeneous solution. The solution was concentrated. The residue was dissolved in chloroform, and the solution was washed with 1N HCl aqueous solution and saturated brine. The organic layer was dried over anhydrous sodium sulfate, and concentrated to obtain yellowish brown crystals (8.9903 g). The product was recrystallized from n-hexane/ethyl acetate to obtain the above-captioned compound ([5]-(54)-278) (7.8455 g) as light yellow crystals.
後処理
- customto obtain a homogeneous solution
- concentrationThe solution was concentrated
- dissolutionThe residue was dissolved in chloroform
- washthe solution was washed with 1N HCl aqueous solution and saturated brine
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-0fecae8b671b4957a472ce0b500305f7
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05731310
関連ノート
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