Potassium Iodide → 2,2',2''-((Ethane-1,1,1-triyltris(benzene-4,1-diyl))tris(oxy))tris(ethan-1-ol)

HRID 539431

반응식

HRID 539431 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)([C:10]2[CH:15]=[CH:14][C:13]([OH:16])=[CH:12][CH:11]=2)[CH3:9])=[CH:4][CH:3]=1.[I-].[K+].C1(=O)[O:30][CH2:29][CH2:28]O1>CN(C=O)C>[OH:1][CH2:2][CH2:3][O:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH2:28][CH2:29][OH:30])=[CH:12][CH:11]=2)([C:17]2[CH:18]=[CH:19][C:20]([O:23][CH2:12][CH2:13][OH:16])=[CH:21][CH:22]=2)[CH3:9])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 7303Ethylene carbonateHCID 931181,1,1-Tris(4-hydroxyphenyl)ethane

생성물 1

HCID 197715052,2',2''-((Ethane-1,1,1-triyltris(benzene-4,1-diyl))tris(oxy))tris(ethan-1-ol)

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
145 °C

실험 절차

A 500 ml round bottom flask is equipped with a mechanical stirrer, thermometer and condenser. Add 50 grams 1,1,1-tris(4-hydroxyphenyl)ethane, 100 grams DMF, 0.5 g. potassium iodide and 47.4 grams of ethylene carbonate. Heat to 145° C. and hold for 6 hours. Add 200 g. ethyl acetate and wash the organic portion four times with 150 g. saturated brine. Strip the solvent from the mix on a rotary evaporator. The yield of tan solid is 78 grams. Recrystallize this crude product by dissolving in 300 g. boiling ethyl acetate and allowing to cool slowly. Collect 70.3 grams of a tan solid; the mp=78-81° C.

후처리

  1. customA 500 ml round bottom flask is equipped with a mechanical stirrer
  2. additionAdd 200 g
  3. washethyl acetate and wash the organic portion four times with 150 g
  4. additionStrip the solvent from the mix on a rotary evaporator
  5. customRecrystallize this crude product
  6. dissolutionby dissolving in 300 g
  7. temperatureto cool slowly
  8. customCollect 70.3 grams of a tan solid

출처 및 근거

ORD 기록
ord-b9d487207dc549e5b7fc9c30c38846bb
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871315B2

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