反応式
[N:1]1([CH2:11][CH2:12][C:13]([OH:15])=O)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1.F[B-](F)(F)F.C1(=O)N(OC(N(C)C)=[N+](C)C)C(=O)CC1.C(N(CC)C(C)C)(C)C.[CH3:45][N:46]([CH3:50])[CH2:47][CH2:48][NH2:49]>CN(C=O)C.[Cl-].[Na+].O>[N:1]1([CH2:11][CH2:12][C:13]([NH:49][CH2:48][CH2:47][N:46]([CH3:50])[CH3:45])=[O:15])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][CH2:2]1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
To a solution of Compound 7 (1.0 g, 4.9 mmol) in DMF (20 mL), 2-succinimido-1,1,3,3-tetramethyluronium tetrafluoroborate (1.8 g, 5.8 mmol) and N,N-diisopropyl ethylamine (1.8 mL, 10.2 mmol) were added. Combined mixture was stirred at room temperature for 30 mins and then a solution of N,N-dimethylethylenediamine (0.64 g, 7.3 mmol) in DMF (2 mL) was added. After stirring the mixture for additional 1 hour, it was poured in brine (100 mL) and extracted with ethyl acetate (2×75 mL). The combined organic layers were washed with brine (3×100 mL) and dried over MgSO4. The solvent was removed under reduced pressure to provide Compound 8 as brown viscous liquid (0.74 g, 55%). This product was used without further purification. The structure of Compound 8 is given below:
後処理
- stirringAfter stirring the mixture for additional 1 hour
- extractionextracted with ethyl acetate (2×75 mL)
- washThe combined organic layers were washed with brine (3×100 mL)
- dry with materialdried over MgSO4
- customThe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-0b949730084b40f59f35c06807c79cf8
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08476443B2
関連ノート
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