Sodium Hydroxide → Chromium(III) 3,5-di-tert-butylsalicylate

HRID 1384768

反応式

HRID 1384768 の反応式
[OH-].[Na+].[C:3]([C:7]1[CH:15]=[C:14]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:13]=[C:9]([C:10]([OH:12])=[O:11])[C:8]=1[OH:20])([CH3:6])([CH3:5])[CH3:4].[Cl-].[Cr+3:22].[Cl-].[Cl-]>O>[C:3]([C:7]1[CH:15]=[C:14]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:13]=[C:9]([C:10]([O-:12])=[O:11])[C:8]=1[OH:20])([CH3:6])([CH3:5])[CH3:4].[Cr+3:22].[C:3]([C:7]1[CH:15]=[C:14]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:13]=[C:9]([C:10]([O-:12])=[O:11])[C:8]=1[OH:20])([CH3:6])([CH3:5])[CH3:4].[C:3]([C:7]1[CH:15]=[C:14]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:13]=[C:9]([C:10]([O-:12])=[O:11])[C:8]=1[OH:20])([CH3:6])([CH3:5])[CH3:4]

参加物

5

反応物 3

HCID 14798Sodium Hydroxide4 回HCID 882083,5-Bis(1,1-dimethylethyl)-2-hydroxybenzoic acid3 回HCID 6452300Chromium(3+) trichloride3 回

生成物 1

HCID 178441095Chromium(III) 3,5-di-tert-butylsalicylate

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

実験手順

450 g of water and 7.2 g of NaOH were placed in a 500-cc beaker, and the mixture was heated under stirring to completely dissolve NaOH. This NaOH aqueous solution was heated to 65° C., and 45 g of 3,5-di-tert-butylsalicylic acid was added thereto under stirring. The mixture was further stirred while keeping the temperature at 65° C. to dissolve 3,5-di-tert-butylsalicylic acid. When pH of the dissolved solution became 6.8, heating and stirring were discontinued, and the solution was filtered to remove insoluble 3,5-di-tert-butylsalicylic acid, thus a brown filtrate being obtained. Separately, 37.2 g of a 40% CrCl3 solution and 120 g of water were placed in a 500-cc beaker to prepare a chromium(III) chloride solution having a pH of 2.1. To this chromium(III) chloride solution was gradually added 120 g of 1% NaOH aqueous solution with spending enough time to obtain a solution of 3.95 in pH. Then, this solution was transferred into a 2-liter beaker, and diluted with water to make the total amount 350 g. This chromium(III) chloride solution was heated to 60° C. and, under stirring, the above-described solution of 3,5-di-tert-butylsalicylic acid kept at 60° C. was dropwise added thereto over a period of time of 1.5 to 2 hours. As the addition proceeded, the reaction solution gradually assumed a light green color. After completion of the dropwise addition, stirring was further continued for 1 hour at a temperature of 60 to 65° C., and the reaction solution was suction filtered and washed with water to obtain 170 g of a reaction product (wet). The pH of the filtrate was 4.00. The reaction product collected by filtration was dried at 50° C. for about 14 hours, and the dried product was pulverized to obtain 70 g of an end product. The reaction product is completely soluble in carbon tetrachloride.

後処理

  1. temperaturethe mixture was heated
  2. stirringThe mixture was further stirred
  3. customat 65° C.
  4. temperatureheating
  5. stirringstirring
  6. filtrationthe solution was filtered
  7. customto remove insoluble 3,5-di-tert-butylsalicylic acid
  8. customthus a brown filtrate being obtained
  9. customto obtain a solution of 3.95 in pH
  10. stirringunder stirring
  11. customkept at 60° C.
  12. additionwas dropwise added
  13. additionAs the addition
  14. additionAfter completion of the dropwise addition
  15. stirringstirring
  16. waitwas further continued for 1 hour at a temperature of 60 to 65° C.
  17. filtrationfiltered
  18. washwashed with water

出典と根拠

ORDレコード
ord-22ab163572814a42a7ed7903e1035dee
出典データセット
uspto-grants-2001_07
特許番号
US06261731B1

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