Acetic Acid → HCID 22329126, 화합물

HRID 586843노트

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HRID 586843 반응식
[C:1](O)(=[O:3])C.C(O)=O.[CH2:8]([O:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[CH:21]=[CH:22][C:23]3[NH:29][CH2:28][CH2:27][C:26]([C:30]([O:32][CH3:33])=[O:31])=[CH:25][C:24]=3[CH:34]=2)=[CH:16][CH:15]=1)[CH3:9]>C1COCC1>[CH2:8]([O:10][CH2:11][CH2:12][O:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]2[CH:21]=[CH:22][C:23]3[N:29]([CH:1]=[O:3])[CH2:28][CH2:27][C:26]([C:30]([O:32][CH3:33])=[O:31])=[CH:25][C:24]=3[CH:34]=2)=[CH:18][CH:19]=1)[CH3:9]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 284Formic AcidHCID 22329032methyl 7-[4-(2-ethoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate

생성물 1

HCID 22329126HCID 22329126, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
50 °C

실험 절차

To anhydrous acetic acid (0.25 ml) was added formic acid (0.13 ml) under ice-cooling, and the mixture was stirred under nitrogen atmosphere at 50° C. for 2 hours. To the mixture was added THF (2 ml) and then was added dropwise, under ice-cooling, a solution of methyl 7-[4-(2-ethoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (0.25 g) in THF (10 ml), and the mixture was stirred at room temperature overnight. The solvent was evaporated, and to the residue was added water. The mixture was extracted with ethyl acetate. The organic layer was washed with sodium hydrogen carbonate solution, water and saturated brine, and dried with anhydrous magnesium sulfate, and the solvent was evaporated to give methyl 7-[4-(2-ethoxyethoxy)phenyl]-1-formyl-2,3-dihydro-1H-1-benzazepine-4-carboxylate (0.2 g) as colorless crystals.

후처리

  1. temperaturecooling
  2. additionwas added dropwise, under ice-
  3. temperaturecooling
  4. customThe solvent was evaporated
  5. additionto the residue was added water
  6. extractionThe mixture was extracted with ethyl acetate
  7. washThe organic layer was washed with sodium hydrogen carbonate solution, water and saturated brine
  8. dry with materialdried with anhydrous magnesium sulfate
  9. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-ddac9a40c8724e6ea2d022ac0aa74ab6
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936602B1

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