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三氟乙酸 → 4'-{[2,4-dioxo-6-(2,2,2-trifluoroethyl)-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl]methyl}biphenyl-2-carbonitrile

HRID 1889340
笔记
打印预览

反应方程式

HRID 1889340 反应方程式
COC1C=C(OC)C=CC=1C[N:6]1[C:11](=[O:12])[C:10]2[CH:13]=[C:14]([CH2:16][C:17]([F:20])([F:19])[F:18])[S:15][C:9]=2[N:8]([CH2:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]3[C:29]([C:34]#[N:35])=[CH:30][CH:31]=[CH:32][CH:33]=3)=[CH:24][CH:23]=2)[C:7]1=[O:36].FC(F)(F)C(O)=O>C1(C)C=CC=CC=1>[O:36]=[C:7]1[N:8]([CH2:21][C:22]2[CH:23]=[CH:24][C:25]([C:28]3[C:29]([C:34]#[N:35])=[CH:30][CH:31]=[CH:32][CH:33]=3)=[CH:26][CH:27]=2)[C:9]2[S:15][C:14]([CH2:16][C:17]([F:20])([F:19])[F:18])=[CH:13][C:10]=2[C:11](=[O:12])[NH:6]1
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

4

反应物 2

HCID 6422三氟乙酸HCID 593515844'-{[3-(2,4-dimethoxybenzyl)-2,4-dioxo-6-(2,2,2-trifluoroethyl)-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl]methyl}biphenyl-2-carbonitrile

产物 1

HCID 593517254'-{[2,4-dioxo-6-(2,2,2-trifluoroethyl)-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl]methyl}biphenyl-2-carbonitrile收率 143.6%

试剂、催化剂与溶剂 1

HCID 1140甲苯溶剂

反应条件

温度
50 °C

实验过程

A mixture of 4′-{[3-(2,4-dimethoxybenzyl)-2,4-dioxo-6-(2,2,2-trifluoroethyl)-3,4-dihydrothieno[2,3-d]pyrimidin-1(2H)-yl]methyl}biphenyl-2-carbonitrile (1.68 g) and trifluoroacetic acid (30 mL) was stirred at 50° C. for 2 hr. To the reaction mixture was added toluene (30 mL), under reduced pressure, and concentrated. The precipitated solid was collected by filtration to give the title compound as a colorless solid (1.8 g, 100%).

后处理

  1. concentrationunder reduced pressure, and concentrated
  2. filtrationThe precipitated solid was collected by filtration

来源与证据

ORD记录
ord-dfac993cf67942ad802555ea05fb7125
来源数据集
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08501750B2

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记