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

HRID 1639028노트

반응식

HRID 1639028 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c6f6f9d33c09402980128e8d2822f939
출처 데이터셋
uspto-grants-1989_11
특허 번호
US04882340

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