Dimethyl Sulfate → [3-(Hydroxymethyl)-2-methoxy-5-methylphenyl]methanol

HRID 1038280

反応式

HRID 1038280 の反応式
[OH:1][CH2:2][C:3]1[C:8]([OH:9])=[C:7]([CH2:10][OH:11])[CH:6]=[C:5]([CH3:12])[CH:4]=1.[OH-].[Na+].S(OC)(O[CH3:19])(=O)=O>O>[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([CH3:12])[CH:6]=[C:7]([CH2:10][OH:11])[C:8]=1[O:9][CH3:19]

参加物

5

反応物 3

HCID 6497Dimethyl Sulfate3 回HCID 70392,6-Dimethylol-p-cresolHCID 14798Sodium Hydroxide

生成物 1

HCID 226768[3-(Hydroxymethyl)-2-methoxy-5-methylphenyl]methanol

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 2,6-bis(hydroxymethyl)-p-cresol (1) (250 g, 1.48 mol), NaOH pellet (90 g, 2.25 mol) in water (2 L), dimethyl sulfate (105 g, 0.84 mol) was added slowly while stirring. The temperature of the reaction mixture was maintained below 40° C. during dimethyl sulfate addition. Copious white precipitate formed upon standing overnight, the white product (150 g) was collected by filtration as the first crop. Dimethyl sulfate (31 g, 0.25 mol) was added to the mother liquor, and the mixture was stirred at room temperature for 5 days. During this time the volume of the mother liquor was reduced to half of its original volume and 70 g of product was collected as the second crop by filtration. Total yield, 220 g (81%).

後処理

  1. customCopious white precipitate formed
  2. filtrationthe white product (150 g) was collected by filtration as the first crop
  3. stirringthe mixture was stirred at room temperature for 5 days
  4. filtrationwas collected as the second crop by filtration

出典と根拠

ORDレコード
ord-68ea383de50340b99cdf8c362fba5b8b
出典データセット
uspto-grants-2013_10
特許番号
US08551453B2

関連ノート

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