Formaldehyde → HCID 20194908, 화합물

HRID 653510노트

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HRID 653510 반응식
[CH3:1][O:2][CH:3]([O:15][CH3:16])[CH2:4][CH2:5][CH:6]([C:11]([O:13][CH3:14])=[O:12])[C:7]([O:9][CH3:10])=[O:8].C=O.[C:19](=O)([O-])[OH:20].[K+]>>[OH:20][CH2:19][C:6]([C:11]([O:13][CH3:14])=[O:12])([C:7]([O:9][CH3:10])=[O:8])[CH2:5][CH2:4][CH:3]([O:2][CH3:1])[O:15][CH3:16]

참가 물질

4

반응물 3

HCID 712FormaldehydeHCID 516893Potassium BicarbonateHCID 13379916Dimethyl (3,3-dimethoxypropyl)propanedioate

생성물 1

HCID 20194908HCID 20194908, 화합물수율 95%

실험 절차

The hydroxymethylation of dimethyl 4,4-dimethoxybutane-1,1-dicarboxylate was carried out. The diester (23.4 g, 0.10 mol) was added dropwise to a mixture of formalin (8.1 ml, 0.10 mol) and potassium hydrogen carbonate (0.8 g, 8 mmol) over 20 min. The mixture was stirred at room temperature for 6 hours until the starting ester was completely consumed. A saturated aqueous solution of ammonium sulfate (35 ml) was added to the reaction mixture. The mixture was then extracted with three 60 ml portions of ethyl ether and the combined extracts were dried over anhydrous magnesium sulfate. The salt was filtered off and rotary evaporation of the solvent from the filtrate gave the product, at 95% yield, as viscous oil.

후처리

  1. customwas completely consumed
  2. additionA saturated aqueous solution of ammonium sulfate (35 ml) was added to the reaction mixture
  3. extractionThe mixture was then extracted with three 60 ml portions of ethyl ether
  4. dry with materialthe combined extracts were dried over anhydrous magnesium sulfate
  5. filtrationThe salt was filtered off
  6. customrotary evaporation of the solvent from the filtrate
  7. customgave the product

출처 및 근거

ORD 기록
ord-0e7c2b7837f24f42b0132d133bab76c9
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04677190

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