Water → 1-Hexylcycloprop-1-ene

In situ, 0.586 g (2.0 mmol) of (trans)-1-hexyl-1-(methane sulfonyloxy)-2-(trimethylsilyl)cyclopropane of Preparation Example 9 was dissolved in 2.0 ml of DMSO, 0.94 g of Bu4NF.3H2O was added thereto and the resulting mixture was vigorously stirred at room temperature for one hour. 8.0 ml of xylene and 5.0 ml of water were added to the reaction solution and vigorously stirred for 5 minutes and stood. When the mixture was separated into a xylene layer (upper layer) and an aqueous layer (lower layer), only the xylene layer was collected and the aqueous layer was discarded. 1.0 g of sodium dodecylbenzenesulfonate and 1.0 g of tristyrenylphenykethoxy)12ethanol were added to the xylene layer, stirred for 5 minutes, 2.0 L of water was added thereto and the resulting mixture was slowly stirred such that it was homogeneously mixed. As a result, a 1.0 mM 1-hexylcyclopropene formulation was prepared. This solution was diluted to 1 to 100 times prior to use, as necessary.

1. stirringvigorously stirred for 5 minutes
2. customWhen the mixture was separated into a xylene layer (upper layer)
3. customan aqueous layer (lower layer), only the xylene layer was collected
4. addition1.0 g of sodium dodecylbenzenesulfonate and 1.0 g of tristyrenylphenykethoxy)12ethanol were added to the xylene layer
5. stirringstirred for 5 minutes
6. addition2.0 L of water was added
7. additionwas homogeneously mixed
8. additionThis solution was diluted to 1 to 100 times

ORDレコード

ord-786126f9c5ea408384c97e7b08a663a8

出典データセット

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09072293B2