4-Hydroxy-2,2,6,6-tetramethylpiperidine → 2,2,6,6-Tetramethylpiperidin-4-yl 2,5-dimethylfuran-3-carboxylate

HRID 746264

반응식

HRID 746264 반응식
[CH3:1][C:2]1[O:3][C:4]([CH3:11])=[CH:5][C:6]=1[C:7]([O:9][CH3:10])=[O:8].OC1[CH2:18][C:17]([CH3:20])([CH3:19])[NH:16][C:15]([CH3:22])([CH3:21])[CH2:14]1>CCCCO.CCCCO.CCCCO.CCCCO.[Ti].CO>[CH3:1][C:2]1[O:3][C:4]([CH3:11])=[CH:5][C:6]=1[C:7]([O:9][CH:10]1[CH2:18][C:17]([CH3:20])([CH3:19])[NH:16][C:15]([CH3:22])([CH3:21])[CH2:14]1)=[O:8]

참가 물질

5

반응물 2

HCID 754714-Hydroxy-2,2,6,6-tetramethylpiperidineHCID 802483-Furancarboxylic acid, 2,5-dimethyl-, methyl ester

생성물 1

HCID 137656342,2,6,6-Tetramethylpiperidin-4-yl 2,5-dimethylfuran-3-carboxylate

시약·촉매·용매 2

HCID 521701Tetrabutoxytitanium촉매HCID 887Methanol용매

실험 절차

154 g (1 mole) of methyl 2,5-dimethylfuran-3-carboxylate and 157 g (1 mole) of 4-hydroxy-2,2,6,6-tetramethylpiperidine were heated together with 10 g of tetrabutyl orthotitanate for 10 hours at about 190° C., the methanol formed being distilled off. When the reaction is complete, the mixture is cooled and the reaction mass is dissolved in ethyl acetate. The solution is extracted by shaking, first with 10% strength sodium carbonate solution and then with water, after which it is dried and evaporated down, and the residue is distilled under reduced pressure. The desired product distils at 142° C./2 mm as a virtually colorless oil which soon solidifies to a solid of melting point 59°-61° C.

후처리

  1. distillationbeing distilled off
  2. temperaturethe mixture is cooled
  3. dissolutionthe reaction mass is dissolved in ethyl acetate
  4. extractionThe solution is extracted
  5. dry with materialwith water, after which it is dried
  6. customevaporated down
  7. distillationthe residue is distilled under reduced pressure
  8. customThe desired product distils at 142° C./2 mm as a virtually colorless oil which

출처 및 근거

ORD 기록
ord-66b19aa7576741619657092ed9d7f36e
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04603205

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