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M-Cresol → Tar acids, methylphenol fraction

HRID 2306527
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HRID 2306527 반응식
[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8].[CH:9]1[C:14]([OH:15])=[CH:13][CH:12]=[C:11]([CH3:16])[CH:10]=1.O.O.C(O)(=O)C(O)=O.C=O>C(C(C)=O)C(C)C.C(OC(C)COC)(=O)C.CCCCCCC.C(O)(=O)C>[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8].[CH:13]1[C:14]([OH:15])=[CH:9][CH:10]=[C:11]([CH3:16])[CH:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 342M-CresolHCID 712FormaldehydeHCID 2879P-CresolHCID 61373Oxalic acid dihydrate

생성물 1

HCID 21829806Tar acids, methylphenol fraction

시약·촉매·용매 4

HCID 176Acetic Acid용매HCID 7909
Methyl Isobutyl Ketone
용매
3회
HCID 7946Propylene glycol methyl ether acetate용매
HCID 8900Heptane용매

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온도
80 °C

실험 절차

Into a 1 L four-necked flask equipped with a reflux tube, stirring apparatus and thermometer were charged 87.3 g of m-cresol, 131.0 g of p-cresol, 6.1 g of oxalic acid dihydrate, 59.3 g of 90% acetic acid and 203 g of methyl isobutyl ketone and the mixture was heated up to 80° C. Into this was dropped 94.2 g of a 37% formaldehyde aqueous solution over 1 hour. Thereafter, the mixture was heated up to reflux temperature and kept at the same temperature for 12 hours. The resulted reaction solution was diluted with methyl isobutyl ketone, and washed with water and dehydrated, to obtain a 38.0% methyl isobutyl ketone solution of a novolak resin. 384 g of this resin solution was charged into a 5 L bottom-discharging type flask, diluted with 574 g of methyl isobutyl ketone, and 764 g of n-heptane was charged and the mixture was stirred at 60° C. and allowed to stand still, then, separated to obtain a novolak resin solution in the lower layer. This novolak resin solution was diluted with propylene glycol methyl ether acetate and then concentrated, to obtain a propylene glycol methyl ether acetate solution of a novolak resin. This resin is called resin A6.

후처리

  1. customInto a 1 L four-necked flask equipped with a reflux tube
  2. temperatureThereafter, the mixture was heated up
  3. temperatureto reflux temperature
  4. customThe resulted reaction solution
  5. washwashed with water
  6. customto obtain a 38.0% methyl isobutyl ketone solution of a novolak resin
  7. additionwas charged
  8. stirringthe mixture was stirred at 60° C.
  9. customseparated
  10. customto obtain a novolak resin solution in the lower layer
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-720a446acbf64bfda60c9983225380eb
출처 데이터셋
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06828079B2

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