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3,4,5-Trimethoxybenzaldehyde → 3,4,5-Trimethoxybenzaldehyde dimethyl acetal

HRID 974108
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인쇄 미리보기

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HRID 974108 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:13][CH3:14])[C:10]=1[O:11][CH3:12])C=O.CO[CH:17]([O:20][CH3:21])[O:18][CH3:19].C[O-].[Na+]>CO.Cl>[CH3:21][O:20][CH:17]([O:18][CH3:19])[C:5]1[CH:8]=[C:9]([O:13][CH3:14])[C:10]([O:11][CH3:12])=[C:3]([O:2][CH3:1])[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 68583,4,5-TrimethoxybenzaldehydeHCID 9005Trimethyl orthoformateHCID 10942334Sodium Methoxide

생성물 1

HCID 41935783,4,5-Trimethoxybenzaldehyde dimethyl acetal수율 100.3%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 887Methanol용매2회

실험 절차

A mixture of 196.2 g of 3,4,5-trimethoxybenzaldehyde, 127.3 g of trimethoxymethane, 200 ml of methanol and 0.1 g of hydrochloric acid is refluxed for 3 hours. After cooling the reaction mixture, 0.2 g of a 24% sodium methoxide solution in methanol is added thereto and the mixture is evaporated under reduced pressure to remove solvent. 150 ml of tetrahydrofuran are added to the residue, and the mixture is evaporated under reduced pressure to remove solvent. 243 g of 3,4,5-trimethoxybenzaldehyde dimethyl acetal are thereby obtained as a pale yellow oil.

후처리

  1. temperatureis refluxed for 3 hours
  2. additionis added
  3. customthe mixture is evaporated under reduced pressure
  4. customto remove solvent
  5. addition150 ml of tetrahydrofuran are added to the residue
  6. customthe mixture is evaporated under reduced pressure
  7. customto remove solvent

출처 및 근거

ORD 기록
ord-eac34bc471ee4134868a9133acfe0832
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05066825

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