反応式
[O:1]=[C:2]1[CH2:7][N:6]([CH2:8][CH2:9][N:10]([CH2:21][C:22]([OH:24])=[O:23])[CH2:11][CH2:12][N:13]2[CH2:18][C:17](=[O:19])[O:16][C:15](=[O:20])[CH2:14]2)[CH2:5][C:4](=[O:25])[O:3]1.[OH2:26].C(N(CC)CC)C.[CH2:34]([O:36][C:37](=[O:49])[CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][NH2:48])[CH3:35]>CN(C)C=O>[C:15]([CH2:14][N:13]([CH2:12][CH2:11][N:10]([CH2:21][C:22]([OH:24])=[O:23])[CH2:9][CH2:8][N:6]([CH2:7][C:2](=[O:1])[NH:48][CH2:47][CH2:46][CH2:45][CH2:44][CH2:43][CH2:42][CH2:41][CH2:40][CH2:39][CH2:38][C:37]([O:36][CH2:34][CH3:35])=[O:49])[CH2:5][C:4]([OH:3])=[O:25])[CH2:18][C:17]([OH:16])=[O:19])([OH:20])=[O:26]参加物
反応条件
- 温度
- 0 °C
実験手順
17.85 g (50 mmol) of 1.5-bis(2,6-dioxomorpholino)-3-carboxymethyl-3-azapentane is stirred in 200 ml of dimethylformamide and mixed with 9 ml (50 mmol) of water. The solution is heated for 3 hours to 70° C., cooled off to 0° C. and 36.07 ml (260 mmol) of triethylamine and 10.8 g (50 mmol) of 11-aminoundecanoic acid ethyl ester are added. After stirring overnight at room temperature, the solution is evaporated to dryness in a vacuum. The residue is taken up in 100 ml of water and the solution is mixed by drops with concentrated hydrochloric acid until permanent cloudiness. After stirring overnight in the ice bath, the finely crystalline precipitate is suctioned off, washed with water and dried in a vacuum at 50° C. 14.9 g (65% of theory) of the title compound is obtained as a white powder with melting point 155-157° C.
後処理
- temperatureThe solution is heated for 3 hours to 70° C.
- customthe solution is evaporated to dryness in a vacuum
- additionthe solution is mixed by drops with concentrated hydrochloric acid until permanent cloudiness
- stirringAfter stirring overnight in the ice bath
- washwashed with water
- customdried in a vacuum at 50° C
出典と根拠
- ORDレコード
- ord-a595cd5bdf54430e8c1443416e011d35
- 出典データセット
- uspto-grants-2003_05
- 特許番号
- US06565830B1
関連ノート
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