反応式
C1(N=C=NC2CCCCC2)CCCCC1.[CH3:16][C:17]1([CH3:26])[C@H:19]([CH:20]=[C:21]=[CH2:22])[C@H:18]1[C:23]([OH:25])=[O:24].[F:27][C:28]1[C:33]([CH2:34]O)=[C:32]([F:36])[C:31]([F:37])=[C:30]([F:38])[C:29]=1[F:39]>C(Cl)Cl.CN(C)C1C=CN=CC=1>[CH3:16][C:17]1([CH3:26])[C@H:19]([CH:20]=[C:21]=[CH2:22])[C@H:18]1[C:23]([O:25][CH2:34][C:33]1[C:32]([F:36])=[C:31]([F:37])[C:30]([F:38])=[C:29]([F:39])[C:28]=1[F:27])=[O:24]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
- 20 °C
実験手順
A solution of 4.12 g of dicyclohexylcarbodiimide in 40 ml of methylene chloride was added at 0° C. to a mixture of 3 g of (1R,trans) 2,2-dimethyl-3-(1,2-propadienyl)-cyclopropane-carboxylic acid, 30 ml of methylene chloride, 3.96 g of pentafluorobenzyl alcohol and 100 mg of 4-dimethylaminopyridine and the mixture was stirred at 20° C. for 16 hours and was filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was chromatographed over silica gel. Elution with a 9-1 hexane-ethyl acetate mixture yielded 4.78 g of pentafluorobenzyl (1R,trans) 2,2-dimethyl-3-(1,2-propadienyl)-cyclopropane-carboxylate with a specific rotation of [α]D20 =-23° (c=0.5% in chloroform).
後処理
- filtrationwas filtered
- customThe filtrate was evaporated to dryness under reduced pressure
- customthe residue was chromatographed over silica gel
- washElution with a 9-1 hexane-ethyl acetate mixture
出典と根拠
- ORDレコード
- ord-45c6e0aa1d6c4d56b6c6cbcaf5f003a5
- 出典データセット
- uspto-grants-1985_08
- 特許番号
- US04537897
関連ノート
読み込み中…