Carbon Dioxide → HCID 178419561、化合物

HRID 449533

反応式

HRID 449533 の反応式
[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

参加物

6

反応物 4

HCID 280Carbon DioxideHCID 6115AnilineHCID 3033972Mucobromic AcidHCID 22137766Aniline ethanol

生成物 1

HCID 178419561HCID 178419561、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-880d2b139b6e475a940ad403434b4ca6
出典データセット
uspto-grants-2013_07
特許番号
US08481752B2

関連ノート

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