Ethylene Glycol → Methyl 5-chloro-3-(1,3-dioxolan-2-yl)-2-hydroxybenzoate

HRID 1761922ノート

反応式

HRID 1761922 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[O:13])[C:5]([OH:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].C[Si](C)(C)Cl.[C:19](=O)(O)[O-].[Na+].CN(C)C.[CH2:28]([OH:31])[CH2:29]O>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]2[O:31][CH2:28][CH2:29][O:13]2)[C:5]([OH:11])=[C:6]([CH:10]=1)[C:7]([O:9][CH3:19])=[O:8]

参加物

6

反応物 5

HCID 174Ethylene GlycolHCID 1146TrimethylamineHCID 6397ChlorotrimethylsilaneHCID 1833565-Chloro-3-formyl-2-hydroxybenzoic acidHCID 516892Sodium Bicarbonate

生成物 1

HCID 19840310Methyl 5-chloro-3-(1,3-dioxolan-2-yl)-2-hydroxybenzoate

実験手順

A mixture of 73.2 g of 5-chloro-3-formyl-2-hydroxybenzoic acid, 350 ml of ethylene glycol and 129 ml of trimethylchlorosilane is stirred at room temperature for 2 hours. The reaction mixture is poured into a mixture of an aqueous saturated sodium bicarbonate solution and trimethylamine, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried and evaporated to remove solvent to give 86 g of methyl 5-chloro-3-(1,3-dioxolan-2-yl)-2-hydroxybenzoate as yellow powder.

後処理

  1. extractionthe mixture is extracted with ethyl acetate
  2. washThe extract is washed with water
  3. customdried
  4. customevaporated
  5. customto remove solvent

出典と根拠

ORDレコード
ord-a37270dc9ce9443c9152c047a73c9e77
出典データセット
uspto-grants-1989_05
特許番号
US04829067

反応ノート

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