二氧化碳 → HCID 178419561，化合物

HRID 449533

反应方程式

HRID 449533 反应方程式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:8](O)(=O)/[C:9](=[C:11](\C=O)/Br)/[Br:10].[NH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(O)C.C(=O)=O>C(O)C>[Br-:10].[Br:10]/[C:9](=[CH:8]\[NH:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)/[CH:11]=[NH+:1]/[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参与物

6

反应物 4

HCID 280二氧化碳HCID 6115苯胺HCID 3033972粘溴酸HCID 22137766Aniline ethanol

产物 1

HCID 178419561HCID 178419561，化合物

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂2 次

实验过程

The procedure as disclosed in the literature (Simonis, H. Ber. Deut. Chem. Ges. 1901, 34, 509; U.S. Pat. No. 6,747,159) is used. 3.54 g of aniline are dissolved in 15 ml of ethanol in a 100 ml beaker. Separately, 5 g of mucobromic acid are dissolved in 15 ml of ethanol in a 100 ml Erlenmeyer flask. This solution is added dropwise to the aniline/ethanol solution, with cooling. The reaction mixture turns immediately yellow, then orange, with development of CO2. At the end of the addition, the mixture is heated in a water bath until its volume is reduced by one half. The resulting solution is cooled with an ice-salt mixture, forming a yellow crystalline precipitate. This solid is collected on a fritted glass filter to afford pure product 5; additional product 5 can be recovered from concentration and recrystallization of the mother liquor.

后处理

  1. temperaturewith cooling
  2. additionAt the end of the addition
  3. temperaturethe mixture is heated in a water bath until its volume
  4. customforming a yellow crystalline precipitate
  5. customThis solid is collected on a fritted glass
  6. filtrationfilter

来源与证据

ORD记录
ord-880d2b139b6e475a940ad403434b4ca6
来源数据集
uspto-grants-2013_07
专利号
US08481752B2

关联笔记

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