海萝胶 → Fluoreneone

HRID 7333

反应方程式

HRID 7333 反应方程式
C(O[C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:15]=[CH:14][C:13](OCCCC)=[C:12](F)[CH:11]=2)=[CH:6][C:5]=1F)C.C([Li])CCC.[C:28](=[O:33])(OC)OC.Cl>CCCCCC.O1CCCC1>[C:28]1(=[O:33])[C:6]2[C:7]([C:10]3[C:11]([CH:5]=2)=[CH:12][CH:13]=[CH:14][CH:15]=3)=[CH:8][CH:9]=[CH:4]1

参与物

7

反应物 4

HCID 313海萝胶HCID 12021碳酸二甲酯HCID 120674464-Ethoxy-3,3'-difluoro-4'-butoxybiphenylHCID 178418339正丁基锂

产物 1

HCID 22281833Fluoreneone

试剂、催化剂与溶剂 2

HCID 8028四氢呋喃溶剂HCID 8058正己烷溶剂

反应条件

温度
-70 °C

实验过程

60 mmol of 4-ethoxy-3,3′-difluoro-4′-butoxybiphenyl (5) are introduced into 200 ml of tetrahydrofuran, and the mixture is cooled to −70° C. 120 mmol of a 1.6 M solution of n-butyllithium in hexane are added dropwise, and the mixture is stirred at this temperature for 2 hours. 60 mmol of dimethyl carbonate are subsequently added rapidly with vigorous stirring, the mixture is stirred at −70° C. for a further hour, allowed to warm to 0° C., hydrolysed with dilute hydrochloric acid and subjected to conventional work-up.

后处理

  1. stirringthe mixture is stirred at −70° C. for a further hour

来源与证据

ORD记录
ord-d72ec14bcd7c4423a145eaa149263f3b
来源数据集
uspto-grants-2006_08
专利号
US07087272B2

关联笔记

加载中…