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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethyl 4-(1-methylpiperidin-4-ylidenemethyl)-3-trifluoromethylbenzoate → HCID 23145989, 화합물

HRID 13759
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HRID 13759 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=[CH:8][C:9]2[CH:19]=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:11][C:10]=2[C:20]([F:23])([F:22])[F:21])[CH2:4][CH2:3]1>CO.[C].[Pd]>[CH3:1][N:2]1[CH2:3][CH2:4][CH:5]([CH2:8][C:9]2[CH:19]=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:11][C:10]=2[C:20]([F:21])([F:23])[F:22])[CH2:6][CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 23145947Ethyl 4-(1-methylpiperidin-4-ylidenemethyl)-3-trifluoromethylbenzoate

생성물 1

HCID 23145989HCID 23145989, 화합물수율 97.5%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

1.57 g of ethyl 4-(1-methylpiperidin-4-ylidenemethyl)-3-trifluoromethylbenzoate (Reference Example 7 (step 2)) was dissolved in 32 ml of methanol and 78 mg of 10% palladium-carbon was added, and then the mixture was hydrogenated at room temperature under 1 atm for 24 hours. The catalyst was removed by filtration and the solvent in the filtrate was distilled off under reduced pressure. The mixture was again dissolved in 32 ml of methanol and 78 mg of 10% palladium-carbon was added thereto, and then the mixture was hydrogenated at room temperature under 1 atm for 4 hours. Further, 78 mg of palladium-carbon was added and the mixture was hydrogenated at room temperature under 1 atm for 24 hours. 78 mg of palladium-carbon was further added and the mixture was hydrogenated at room temperature under 1 atm for 19 hours. The catalyst was removed by filtration and the solvent in the filtrate was distilled off under reduced pressure to obtain 1.54 g of the objective compound as a green oily product.

후처리

  1. customThe catalyst was removed by filtration
  2. distillationthe solvent in the filtrate was distilled off under reduced pressure
  3. dissolutionThe mixture was again dissolved in 32 ml of methanol
  4. addition78 mg of 10% palladium-carbon was added
  5. waitthe mixture was hydrogenated at room temperature under 1 atm for 4 hours
  6. additionFurther, 78 mg of palladium-carbon was added
  7. waitthe mixture was hydrogenated at room temperature under 1 atm for 24 hours
  8. addition78 mg of palladium-carbon was further added
  9. waitthe mixture was hydrogenated at room temperature under 1 atm for 19 hours
  10. customThe catalyst was removed by filtration
  11. distillationthe solvent in the filtrate was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-b87d3e90aa3b47fb81c02b98cb9a9544
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07728131B2

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