M-Cresol → 2-Hydroxy-6-methylbenzaldehyde

HRID 37032

反応式

HRID 37032 の反応式
[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]

参加物

7

反応物 5

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

生成物 1

HCID 5851742-Hydroxy-6-methylbenzaldehyde

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

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 97 percent pure 2,6-bis(hydroxy-methyl)-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-cresolformaldehyde 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.

後処理

  1. customwas formed
  2. additionin a solvent mixture of 40 ml
  3. customforming the alternating copolymer
  4. customAt 102° C

出典と根拠

ORDレコード
ord-686f17f2d5d543edaf3ff1637021c425
出典データセット
uspto-grants-1995_05
特許番号
US05419995

関連ノート

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