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Sulfuric Acid → Methacrylamidopropyldimethyl-2,3-dihydroxypropylammonium sulfate

HRID 568961
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HRID 568961 반응식
[CH3:1][C:2]([C:4]([NH:6][CH2:7][CH2:8][CH2:9][N:10]([CH3:12])[CH3:11])=[O:5])=[CH2:3].[CH2:13]1[O:15][CH:14]1[CH2:16][OH:17].[OH:18][S:19]([OH:22])(=[O:21])=[O:20]>O>[S:19]([O-:22])([O-:21])(=[O:20])=[O:18].[C:4]([NH:6][CH2:7][CH2:8][CH2:9][N+:10]([CH3:12])([CH3:11])[CH2:13][CH:14]([OH:15])[CH2:16][OH:17])(=[O:5])[C:2]([CH3:3])=[CH2:1].[C:4]([NH:6][CH2:7][CH2:8][CH2:9][N+:10]([CH2:13][CH:14]([OH:15])[CH2:16][OH:17])([CH3:12])[CH3:11])(=[O:5])[C:2]([CH3:1])=[CH2:3]
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참가 물질

5

반응물 3

HCID 1118Sulfuric Acid3회HCID 11164Glycidol4회HCID 78882N-(3-(Dimethylamino)propyl)methacrylamide

생성물 1

HCID 14093557Methacrylamidopropyldimethyl-2,3-dihydroxypropylammonium sulfate

시약·촉매·용매 1

HCID 962Water용매2회

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온도
40 °C

실험 절차

To a 1-liter glass beaker containing a magnetic stirrer is added 170.26 g (1 mole) of DMAPMA and 170.26 of deionized water while stirring. Initial pH and temperature are 11.2 and 23.1° C., respectively. Two addition funnels are suspended above the beaker; one contains 75.6 g (1 mole) of glycidol and the other contains 98.2 g of 50% H2SO4. The pH and temperature are monitored continuously during the drop-wise addition of glycidol. Temperature is maintained between 19.5° and 27.5° C. by placing the beaker in an ice bath. The pH is maintained between 10.6 and 11.2 by adding 50% H2SO4 as needed. All of the glycidol is added within 1 hour and 4 minutes. An additional 75.6 g of water is added to the reaction mixture; a portion is flowed through the addition funnel which contained the glycidol and the remainder is added to the addition funnel containing the remaining H2SO4. The ice bath surrounding the reaction vessel is removed and replaced with a warm water bath in order to raise the reaction temperature to 40° C. The remaining acid and water mixture is added to the reaction vessel over a period of 2 hours and 41 minutes. During this stepwise addition the temperature is held at about 40° C. and the pH is maintained between 11.3 and 10.1 until the last portion of acid is added. The final pH is 4.55. The reaction mixture is then placed in a sealed brown bottle and submerged in a 42° C. bath. The reaction mixture is removed at 16 hours. The final pH of the product is 5.2 at room temperature.

후처리

  1. custom11.2 and 23.1° C.
  2. additionTwo addition funnels
  3. temperatureTemperature is maintained between 19.5° and 27.5° C.
  4. temperatureThe pH is maintained between 10.6 and 11.2
  5. additionthe remainder is added to the addition funnel
  6. customis removed
  7. customreplaced with a warm water bath in order
  8. additionThe remaining acid and water mixture is added to the reaction vessel over a period of 2 hours and 41 minutes
  9. additionDuring this stepwise addition the temperature
  10. customis held at about 40° C.
  11. temperaturethe pH is maintained between 11.3 and 10.1 until the last portion of acid
  12. additionis added
  13. customsubmerged in a 42° C.
  14. customThe reaction mixture is removed at 16 hours
  15. customat room temperature

출처 및 근거

ORD 기록
ord-62c56c3ff1a54c708e8f4ce32a84850e
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04730081

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