Water → HCID 25151661、化合物
反応式
N[CH:2]([OH:4])[CH3:3].Br[CH2:6][C:7]1[C:8](=[O:36])[N:9]([C:13]2[CH:18]=[CH:17][C:16]([N:19]3[CH2:23][C@H:22]([CH2:24][NH:25][C:26]([C:28]4[S:29][C:30]([Cl:33])=[CH:31][CH:32]=4)=[O:27])[O:21][C:20]3=[O:34])=[CH:15][C:14]=2[CH3:35])[CH:10]=[CH:11][CH:12]=1.O.C[N:39](C=O)C>>[Cl:33][C:30]1[S:29][C:28]([C:26]([NH:25][CH2:24][C@@H:22]2[O:21][C:20](=[O:34])[N:19]([C:16]3[CH:17]=[CH:18][C:13]([N:9]4[CH:10]=[CH:11][CH:12]=[C:7]([CH2:6][NH:39][CH2:3][CH2:2][OH:4])[C:8]4=[O:36])=[C:14]([CH3:35])[CH:15]=3)[CH2:23]2)=[O:27])=[CH:32][CH:31]=1参加物
5
実験手順
At −10° C., 38 mg (0.63 mmol) of aminoethanol are added to a solution of 56 mg (0.11 mmol) of the compound from Example 11A in 1 ml of DMF. After 30 min at −10° C., the mixture is added to water and then extracted three times with ethyl acetate. The organic phases are combined and then freed from the solvent under reduced pressure. The product is purified by preparative HPLC using an acetonitrile/water mixture. This gives 14.5 mg (26% of theory) of the desired product.
後処理
- extractionextracted three times with ethyl acetate
- customThe product is purified by preparative HPLC
出典と根拠
- ORDレコード
- ord-7cb27ad1f88f4a799e5ba175d9964c5c
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08383822B2
反応ノート
読み込み中…