反応式
[C:1]([NH:8][CH2:9][C:10]([OH:12])=[O:11])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].O[N:14]1[C:18](=[O:19])[CH2:17][CH2:16][C:15]1=[O:20].C1(N=C=NC2CCCCC2)CCCCC1>C(Cl)Cl>[C:4]([O:3][C:1]([NH:8][CH2:9][C:10]([O:12][N:14]1[C:18](=[O:19])[CH2:17][CH2:16][C:15]1=[O:20])=[O:11])=[O:2])([CH3:6])([CH3:7])[CH3:5]参加物
5
実験手順
N-Boc-glycine (7.31 g, 41.7 mmol) was dissolved in 100 mL of DCM and to the cooled (15° C.) solution N-hydroxysuccinimide (5.28 g, 45.9 mmol) was added. N,N′-dicyclohexylcarbodiimide (9.47 g, 45.9 mmol) was added to the formed suspension under vigorous stirring. After a few seconds, a cloudy white suspension formed, the mixture was allowed to reach room temperature and stirred for 1 h. It was subsequently filtrated over celite, washed with 50 mL saturated sodium bicarbonate, dried over sodium sulfate and concentrated in vacuo to yield a crystalline powder. Yield: 7.02 g, 61.8%
後処理
- additionwas added
- waitAfter a few seconds
- customa cloudy white suspension formed
- customto reach room temperature
- filtrationIt was subsequently filtrated over celite
- washwashed with 50 mL saturated sodium bicarbonate
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customto yield a crystalline powder
出典と根拠
- ORDレコード
- ord-5de66e3e0b704fb984cf6ce0ec846149
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09346814B2
関連ノート
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