反応式
[CH3:1][O:2][C:3]([C:5]1[N:6]([NH:10][C:11](=[O:21])[CH2:12][O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:7]=[N:8][CH:9]=1)=[O:4].[CH2:22](OC(C)C(O)=O)C1C=CC=CC=1.CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C1COCC1.O>[CH3:1][O:2][C:3]([C:5]1[N:6]([NH:10][C:11](=[O:21])[CH:12]([O:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH3:22])[CH:7]=[N:8][CH:9]=1)=[O:4]参加物
8
反応物 4
生成物 1
試薬・触媒・溶媒 3
実験手順
To a solution of compound 2 (4.2 g, 29.7 mmol), 2-Benzyloxy-propionic acid (5.5 g, 29.7 mmol) and DIEA (10 mL) in a mixture of DMF (1 mL) and THF (50 mL) in ice-water bath was added HATU (13.5 g, 35.7 mmol). The resulting mixture was then stirred at ambient temperature overnight. Water (100 mL) was added. The mixture was extracted with ethyl acetate (300 mL×2). The combined organic phases were concentrated to give a crude residue, which was purified by chromatography on silica gel column (eluted with PE/EtOAc=1:1 to 1:3) to afford compound 9 (8.2 g, 91% yield) as brown oil. LC-MS: m/z 304 [M+H]+.
後処理
- extractionThe mixture was extracted with ethyl acetate (300 mL×2)
- concentrationThe combined organic phases were concentrated
- customto give a crude residue, which
- customwas purified by chromatography on silica gel column (eluted with PE/EtOAc=1:1 to 1:3)
出典と根拠
- ORDレコード
- ord-efc87d032fbe4100bf345dd07e40e300
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434733B2
関連ノート
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