Methacryloyl chloride → 1,2,3-Benzenetricarboxylic acid

HRID 61321

反応式

HRID 61321 の反応式
[OH-].[Na+].N[C:4]1[CH:9]=[C:8]([C:10]([OH:12])=[O:11])[C:7]([C:13]([OH:15])=[O:14])=[C:6]([C:16]([OH:18])=[O:17])[CH:5]=1.C(Cl)(=O)C(C)=C.Cl(O)(=O)=O>O>[C:6]1([C:16]([OH:18])=[O:17])[CH:5]=[CH:4][CH:9]=[C:8]([C:10]([OH:12])=[O:11])[C:7]=1[C:13]([OH:15])=[O:14]

参加物

6

反応物 4

HCID 13528Methacryloyl chloride3 回HCID 14798Sodium Hydroxide2 回HCID 19654Chloric acidHCID 144348615-Amino-1,2,3-benzenetricarboxylic acid

生成物 1

HCID 112881,2,3-Benzenetricarboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
10 °C

実験手順

A 2 litter flask equipped with a magnetic stirrer, a thermometer, and 250 ml dripping funnel were filled with 1 litter of water and 71 g of sodium hydroxide pellet. When this was dissolved, 100 g of 1-aminobenzene-3,4,5-tricarboxylic acid was added and dissolved. After neutralization heat ceased, the reaction result was cooled down to 10° C. The dripping funnel was filled with 40.23 g of methacryloyl chloride. While this was maintained below 15° C., the liquid was dripped to the reaction container in 15 minutes. 40 g of sodium hydroxide was dissolved in 150 g of water in another container. This solution was added to the reaction mixture 20 minutes after the addition of methacryloyl chloride was complete. After the reaction product was cooled down to 10° C., 40 g of methacryloyl chloride was dripped from the dripping funnel in 15 minutes while the temperature was maintained below 15° C. 20 minutes after the dripping was complete, the reaction mixture was acidized to pH 3 by strong chloric acid. The thus-produced solid portion was extracted by vacuum filtration followed by washing with ethanol and dried at 60° C. for 14 hours in a vacuum oven.

後処理

  1. customA 2 litter flask equipped with a magnetic stirrer
  2. dissolutionWhen this was dissolved
  3. dissolutiondissolved
  4. temperatureAfter neutralization heat
  5. customthe reaction result
  6. temperatureWhile this was maintained below 15° C.
  7. additionThis solution was added to the reaction mixture 20 minutes
  8. temperatureAfter the reaction product was cooled down to 10° C.
  9. temperaturewas maintained below 15° C
  10. custom20 minutes
  11. extractionThe thus-produced solid portion was extracted by vacuum filtration
  12. washby washing with ethanol
  13. customdried at 60° C. for 14 hours in a vacuum oven

出典と根拠

ORDレコード
ord-da715e30b7b54c4082e65d2c95077131
出典データセット
uspto-grants-2016_09
特許番号
US09441129B2

関連ノート

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