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Potassium Hydroxide → Diglycidyl ether

HRID 404308
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HRID 404308 반응식
C[C@H]1CO[C@@]2([O:9][C@H]3C[C@H]4[C@@H]5CC=C6C[C@@H](O)CC[C@]6(C)[C@H]5CC[C@]4(C)[C@H]3[C@@H]2C)CC1.[OH-].[K+].[CH2:33]([O:37][CH2:38][CH2:39][CH2:40]CCCCCCCCC)[CH:34]1[O:36][CH2:35]1>C1(C)C=CC=CC=1>[CH2:38]([O:37][CH2:33][CH:34]1[O:36][CH2:35]1)[CH:39]1[O:9][CH2:40]1
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참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 171631-Dodecyl glycidyl etherHCID 99474Diosgenin

생성물 1

HCID 16704Diglycidyl ether

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
60 °C

실험 절차

In a 250 mL, round bottom 3-neck flask equipped with a condenser, a nitrogen in/out let, a mechanical stirrer, a thermo-watch, and a heating mantle, a mixture of 30 g of 10,000 Mw PEG and toluene (80 mL) was heated to 60° C. At this temperature, KOH (2.19 g, 0.04 mol, in 2 g of water) was added and the reaction mixture was stirred for 1 hour. Dodecyl glycidyl ether (8.71 g, 0.04 mole) was added and the reaction temperature was kept at 110° C. for 5 hours. After the reaction mass was cooled to 60° C., toluene (80 mL) was further added. The solution was precipitated into 300 mL of hexane. After filtration and washing with ethyl acetate (100 mL×3×) and drying in vaccuo, a white polymer (33 g) was obtained. 1H NMR showed 11% hydrophobe incorporation. The Brookfield viscosity of a 5% aqueous solution of this oligomer was >200,000 cps (BF LV, S-63, 0.3 rpm at 25° C.). Paint performance: SG10 M (standard formulation). The material was not soluble in this paint. For UCAR 379 G, TE %=0.52, VLT=−6 KU.

후처리

  1. customIn a 250 mL, round bottom 3-neck flask equipped with a condenser
  2. waitthe reaction temperature was kept at 110° C. for 5 hours
  3. temperatureAfter the reaction mass was cooled to 60° C.
  4. customThe solution was precipitated into 300 mL of hexane
  5. filtrationAfter filtration
  6. washwashing with ethyl acetate (100 mL×3×)
  7. customdrying in vaccuo

출처 및 근거

ORD 기록
ord-3d52e44e7d7a421fb1f5ebc412838b1e
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08748542B2

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