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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethylene Oxide → HCID 21997101, 화합물

HRID 1976999
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HRID 1976999 반응식
[F:1][C:2]([F:15])([F:14])[C:3]1([C:10](F)(F)F)[O:7][CH:6]([CH2:8][OH:9])[CH2:5][O:4]1.C1OC1C.[OH-].[K+].C1OC1>>[CH3:10][C:3]1([C:2]([F:15])([F:1])[F:14])[O:7][CH:6]([CH2:8][OH:9])[CH2:5][O:4]1
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참가 물질

5

반응물 4

HCID 6354Ethylene OxideHCID 6378Propylene OxideHCID 14797Potassium HydroxideHCID 219971032,2-Bis(trifluoromethyl)-4-hydroxymethyl-1,3-dioxolane

생성물 1

HCID 21997101HCID 21997101, 화합물

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온도
125 °C

실험 절차

A 2 L stirrer-equipped autoclave was charged with 2,2-bis(trifluoromethyl)-4-hydroxymethyl-1,3-dioxolane (96.1 g; 0.4 moles), propylene oxide (23.3 g; 0.4 moles), and potassium hydroxide (0.6 g). The autoclave was purged of oxygen using argon gas and then sealed. While stirring the mixture, the temperature of the autoclave was raised to 125° C. and then kept at that temperature for 3 hours. After cooling the mixture to room temperature, the autoclave was vented. Next, ethylene oxide (52.9 g; 1.2 moles) was condensed at 0° C. into the mixture with stirring. While continuing to cool the combined mixture, the autoclave was again purged of oxygen using argon gas and then sealed. While stirring the mixture, the temperature of the autoclave was raised to 130° C. and then kept at that temperature for 3 hours. After cooling the mixture to room temperature, the autoclave was vented and the crude product was transferred to a 300 mL round bottom flask. Pure product was isolated by vacuum distillation at 186° C. and 0.3 mm of Hg. The yield of product was 143 g which is 83% of the theoretical value. In the examples and test evaluations described below, this compound is abbreviated (F3)(F3)-ipg-(PO)(EO)3.

후처리

  1. customA 2 L stirrer-equipped autoclave
  2. customThe autoclave was purged of oxygen
  3. customsealed
  4. temperatureAfter cooling the mixture to room temperature
  5. customcondensed at 0° C. into the mixture
  6. stirringwith stirring
  7. temperatureto cool the combined mixture
  8. customthe autoclave was again purged of oxygen
  9. customsealed
  10. stirringWhile stirring the mixture
  11. temperaturethe temperature of the autoclave was raised to 130° C.
  12. waitkept at that temperature for 3 hours
  13. temperatureAfter cooling the mixture to room temperature
  14. customthe crude product was transferred to a 300 mL round bottom flask
  15. customPure product was isolated by vacuum distillation at 186° C.

출처 및 근거

ORD 기록
ord-84f2f51a6e124a4abc0910fedcff026d
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06231655B1

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