Ammonia → 4-Hydroxymethyl-2,5-dimethylphenol

HRID 361973

反応式

HRID 361973 の反応式
[C:1]1([OH:9])[C:2]([CH3:8])=[CH:3][CH:4]=[C:5]([CH3:7])[CH:6]=1.[OH-:10].[Na+].[CH2:12]=O.N>C(O)(=O)C.O>[OH:10][CH2:12][C:4]1[C:5]([CH3:7])=[CH:6][C:1]([OH:9])=[C:2]([CH3:8])[CH:3]=1

参加物

7

反応物 4

HCID 222AmmoniaHCID 712FormaldehydeHCID 72672,5-DimethylphenolHCID 14798Sodium Hydroxide

生成物 1

HCID 109426404-Hydroxymethyl-2,5-dimethylphenol

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

反応条件

温度
12 °C

実験手順

Into a 5 liter four-necked flask were charged 610.9 g of 2,5-xylenol, 200 gof sodium hydroxide and 2500 g of water. While stirring at 12° C., 565 g of 37% formaldehyde was added dropwise thereto over 1 hour and 30 minutes, and the reaction was conducted for 4 more hours. After completionof the reaction, 89 g of 28% aqueous ammonia solution was added and the mixture was stirred for 30 minutes. Thereafter, 400 g of acetic acid was added thereto, and the resulting mixture was filtered and washed with water. The filtered product thus obtained was dried to obtain 609 g of 4-hydroxymethyl-2,5-dimethylphenol. Purity measured by liquid chromatography (LC): 99%

後処理

  1. custom30 minutes
  2. additionwas added
  3. stirringthe mixture was stirred for 30 minutes
  4. filtrationthe resulting mixture was filtered
  5. washwashed with water
  6. customThe filtered product thus obtained
  7. customwas dried

出典と根拠

ORDレコード
ord-78fd208b70014bb693819b515af4127a
出典データセット
uspto-grants-1999_02
特許番号
US05866724

関連ノート

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