反応式
C1(N=C=NC2CCCCC2)CCCCC1.[CH3:16][C:17]1([CH3:33])[C@@H:19]([C:20]#[C:21][C:22]([O:24][CH:25]2[CH2:29][CH2:28][CH2:27][CH2:26]2)=[O:23])[C@H:18]1[C:30]([OH:32])=[O:31].[C:34]([C@@H:36](O)[C:37]1[CH:42]=[CH:41][CH:40]=[C:39]([O:43][C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)[CH:38]=1)#[N:35]>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:16][C:17]1([CH3:33])[C@@H:19]([C:20]#[C:21][C:22]([O:24][CH:25]2[CH2:26][CH2:27][CH2:28][CH2:29]2)=[O:23])[C@H:18]1[C:30]([O:32][C@H:36]([C:34]#[N:35])[C:37]1[CH:42]=[CH:41][CH:40]=[C:39]([O:43][C:44]2[CH:45]=[CH:46][CH:47]=[CH:48][CH:49]=2)[CH:38]=1)=[O:31]参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 0 °C
実験手順
2.96 g of dicyclohexylcarbodiimide were added at 0° C. to a stirred mixture of 3.6 g of the product of Step B, 30 ml of methylene chloride and 30 mg of 4-dimethylaminopyridine followed by the addition of a solution of 3.3 g of (S)α-cyano-3-phenoxy-benzyl alcohol in 10 ml of methylene chloride. The mixture was stirred at 0° C. for 5 minutes and at 20°-25° C. for 3 hours and was filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with a cyclohexane-ethyl acetate mixture yielded 4.5 g of (S)α-cyano-3-phenoxybenzyl(1R,cis)2,2-dimethyl-3-[2-(cyclopentyloxycarbonyl)ethynyl]-cyclopropane-carboxylate with a melting point of =72° C.
後処理
- filtrationwas filtered
- customThe filtrate was evaporated to dryness under reduced pressure
- customthe residue was chromatographed over silica gel
- washElution with a cyclohexane-ethyl acetate mixture
出典と根拠
- ORDレコード
- ord-35cc5308e291490b9e64da0d0b9a6f79
- 出典データセット
- uspto-grants-1985_10
- 特許番号
- US04547522
関連ノート
読み込み中…