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M-Cresol → Tar acids, methylphenol fraction

HRID 2306527
ノート
印刷プレビュー

反応式

HRID 2306527 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

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

生成物 1

HCID 21829806Tar acids, methylphenol fraction

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒HCID 7909
Methyl Isobutyl Ketone
溶媒
3 回
HCID 7946Propylene glycol methyl ether acetate溶媒
HCID 8900Heptane溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-720a446acbf64bfda60c9983225380eb
出典データセット
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06828079B2

反応ノート

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