M-Cresol → 2-Hydroxy-6-methylbenzaldehyde

HRID 260629

반응식

HRID 260629 반응식
[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8].[OH:9][CH2:10]C1C(O)=C(CO)C=C(C)C=1.O.O.C(O)(=O)C(O)=O.CCOCCOC(C)=O.C=O>O>[C:1]1([CH:10]=[O:9])[C:2]([CH3:8])=[CH:3][CH:4]=[CH:5][C:6]=1[OH:7]

참가 물질

7

반응물 5

HCID 342M-CresolHCID 712FormaldehydeHCID 70392,6-Dimethylol-p-cresolHCID 8095Glycol monoethyl ether acetateHCID 61373Oxalic acid dihydrate

생성물 1

HCID 5851742-Hydroxy-6-methylbenzaldehyde

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

A phenolic resin rich in alternating phenolic copolymer block segments was formed by reacting a mixture of 519.0 g of 99 percent pure m-cresol, 538.2 g of 97 percent pure 2,6-bis(hydroxymethyl)-p-cresol and 20 g oxalic acid dihydrate in a solvent mixture of 40 ml deionized water and 200 ml ethyl cellosolve acetate. The reaction mixture was heated to about 70° C. to initiate the reaction forming the alternating copolymer. At 102° C., 32.6 g of 36.9 percent formaldehyde was added in 8 minutes to the reaction mixture to form substantially m-cresol formaldehyde block segments and to chemically bond these segments to the previously formed alternating copolymer. After heating the mixture at reflux for three hours, the amount of heat was increased to remove the water and solvent by distillation. Partial vacuum was applied at about 220° C. and gradually increased to 4 mm Hg to remove the unreacted monomers. Maximum mixture temperature during vacuum stripping was about 226° C. The copolymer was poured from the reaction kettle and allowed to cool. About 840 g of a block copolymer having a number average molecular weight number, Mn, of 1241 Daltons and a Tg of 112° C. were obtained.

후처리

  1. customwas formed
  2. additionin a solvent mixture of 40 ml
  3. customforming the alternating copolymer

출처 및 근거

ORD 기록
ord-cb9a12a81655484faf2860ad4adbd1e8
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05529880

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