反応式
CC([O:5][C:6](=[O:36])[CH2:7][N:8]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15][N:14]([CH2:20][C:21]([O:23]C(C)(C)C)=[O:22])[CH2:13][CH2:12][N:11]([CH2:28][C:29]([O:31]C(C)(C)C)=[O:30])[CH2:10][CH2:9]1)(C)C.Br[CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH3:55]>CC#N>[CH2:55]([N:17]1[CH2:16][CH2:15][N:14]([CH2:20][C:21]([OH:23])=[O:22])[CH2:13][CH2:12][N:11]([CH2:28][C:29]([OH:31])=[O:30])[CH2:10][CH2:9][N:8]([CH2:7][C:6]([OH:5])=[O:36])[CH2:19][CH2:18]1)[CH2:54][CH2:53][CH2:52][CH2:51][CH2:50][CH2:49][CH2:48][CH2:47][CH2:46][CH2:45][CH2:44][CH2:43][CH2:42][CH2:41][CH2:40][CH2:39][CH3:38]参加物
4
実験手順
A mixture of 1,4,7,10-tetraazacyclododecane-1,4,7-triacetic acid tris(1,1-dimethylethyl)ester (37.5 g; 72.8 mmol) and 1-bromooctadecane (24.5 g; 73.5 mmol) in CH3CN (500 mL) was heated to reflux. After 2 h the reaction mixture was evaporated and the residue was dissolved in CHCl3 and a portion of CF3COOH was added. After 16 h at room temperature the reaction mixture was evaporated and the oily residue dissolved in CF3COOH. After 3 days at room temperature, the solution was evaporated, the residue taken up in CHCl3 and the solution evaporated. This operation was repeated three times. The oily residue was purified by flash chromatography as follows:
後処理
- temperaturewas heated to reflux
- customAfter 2 h the reaction mixture was evaporated
- dissolutionthe residue was dissolved in CHCl3
- additiona portion of CF3COOH was added
- customAfter 16 h at room temperature the reaction mixture was evaporated
- dissolutionthe oily residue dissolved in CF3COOH
- customthe solution was evaporated
- customthe solution evaporated
- customThe oily residue was purified by flash chromatography
出典と根拠
- ORDレコード
- ord-a664bd2018a943e3a5baf1503454e641
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06652834B2
関連ノート
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