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Potassium Iodide → HCID 18538872, 화합물

HRID 412937
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HRID 412937 반응식
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH3:8][C:9]1[S:13][C:12]([S:14][CH:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)=[N:11][N:10]=1.[C:21]([N:24]1[CH2:29][CH2:28][CH:27]([C:30]([N:32]([C:37]2[CH:42]=[CH:41][CH:40]=[C:39]([Cl:43])[CH:38]=2)[CH2:33][CH2:34][CH2:35]Cl)=[O:31])[CH2:26][CH2:25]1)(=[O:23])[CH3:22].C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[Cl-].[Na+]>C(#N)C>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[C:21]([N:24]1[CH2:29][CH2:28][CH:27]([C:30]([N:32]([C:37]2[CH:42]=[CH:41][CH:40]=[C:39]([Cl:43])[CH:38]=2)[CH2:33][CH2:34][CH2:35][N:18]2[CH2:19][CH2:20][CH:15]([S:14][C:12]3[S:13][C:9]([CH3:8])=[N:10][N:11]=3)[CH2:16][CH2:17]2)=[O:31])[CH2:26][CH2:25]1)(=[O:23])[CH3:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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7

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HCID 4875Potassium IodideHCID 5234Sodium ChlorideHCID 11430Potassium CarbonateHCID 18538456HCID 18538456, 화합물HCID 18538476HCID 18538476, 화합물

생성물 1

HCID 18538872HCID 18538872, 화합물

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매

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온도
80 °C

실험 절차

4-(5-Methyl-1,3,4-thiadiazol-2-ylthio)piperidine trifluoroacetate (59 mg, 0.18 mmol) was dissolved in dry acetonitrile (1.5 mL). To the solution were added 1-acetyl-N-(3-chlorophenyl)-N-(3-chloropropyl)-4-piperidinecarboxamide (50 mg, 0.14 mmol), potassium carbonate (77 mg, 0.56 mmol) and potassium iodide (23 mg, 0.14 mmol), and the mixture was stirred at 80° C. for 5 hours. The mixture was cooled to room temperature, and to the mixture was added saturated sodium chloride solution (3 mL). The mixture was extracted three times with ethyl acetate (2 mL). The extracts were combined and concentrated under reduced pressure. The concentrate was purified by using HPLC to give the titled compound as a colorless oily substance (32.2 mg, 28%).

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. extractionThe mixture was extracted three times with ethyl acetate (2 mL)
  3. concentrationconcentrated under reduced pressure
  4. customThe concentrate was purified

출처 및 근거

ORD 기록
ord-2ebd06ffe6e7402898b28e7a1016bd76
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06562978B1

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