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

HRID 1639028ノート

反応式

HRID 1639028 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:13]=[O:14])[C:5]([OH:12])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].C[Si](C)(C)Cl.[C:20](=[O:23])(O)[O-].[Na+].[CH3:25]N(C)C>C(O)CO>[Cl:1][C:2]1[CH:11]=[C:6]([CH:7]2[O:8][CH2:25][CH2:10][O:9]2)[C:5]([OH:12])=[C:4]([CH:3]=1)[C:13]([O:23][CH3:20])=[O:14]

参加物

6

反応物 4

HCID 1146TrimethylamineHCID 6397ChlorotrimethylsilaneHCID 516892Sodium BicarbonateHCID 13146779Methyl 5-chloro-3-formyl-2-hydroxybenzoate

生成物 1

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

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

A mixture of methyl 5-chloro-3-formyl-2-hydroxybenzoate (73.2 g), ethylene glycol (350 ml) and trimethylchlorosilane (129 ml) 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 extracted is washed with water, dried and concentrated to remove solvent, whereby methyl 5-chloro-3-(1,3-dioxolan-2-yl)-2-hydroxybenzoate (86 g) is obtained as yellow powder.

後処理

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

出典と根拠

ORDレコード
ord-c6f6f9d33c09402980128e8d2822f939
出典データセット
uspto-grants-1989_11
特許番号
US04882340

反応ノート

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