Sulfuric Acid → 4'-(Hydroxymethyl)-[1,1'-Biphenyl]-2-Carboxylic Acid

HRID 742796

反応式

HRID 742796 の反応式
S(=O)(=O)(O)O.CC1(C)C[O:10][C:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[C:18]2[CH:23]=[CH:22][C:21]([CH2:24][OH:25])=[CH:20][CH:19]=2)=N1.[OH-:27].[Na+]>O>[OH:25][CH2:24][C:21]1[CH:22]=[CH:23][C:18]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[C:9]([OH:10])=[O:27])=[CH:19][CH:20]=1

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 110658764,4-Dimethyl-2-(4'hydroxymethylbiphenyl-2-yl)oxazoline

生成物 1

HCID 153808804'-(Hydroxymethyl)-[1,1'-Biphenyl]-2-Carboxylic Acid収率 65%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Water (6 ml) and sulfuric acid (3.6 g) were added to 2.0 g (7.11 mmol) of 4,4-dimethyl-2-(4'-hydroxymethylbiphenyl-2-yl)oxazoline, followed by heating under reflux for 30 hours. After the reaction liquid was cooled, it was neutralized with a 10% aqueous solution of sodium hydroxide and extracted with chloroform. After the organic phase was washed with water and dried, it was subjected to vacuum concentration. The residue was purified by silica gel column chromatography (a chloroform/methanol system) to give 1.05 g of the title compound (yield 65%).

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 30 hours
  3. customAfter the reaction liquid
  4. temperaturewas cooled
  5. extractionextracted with chloroform
  6. washAfter the organic phase was washed with water
  7. customdried
  8. concentrationit was subjected to vacuum concentration
  9. customThe residue was purified by silica gel column chromatography (a chloroform/methanol system)

出典と根拠

ORDレコード
ord-4a91a79bf803431684faf00f59b512a7
出典データセット
uspto-grants-1996_09
特許番号
US05554757

関連ノート

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