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Potassium Iodide → HCID 18538984、化合物

HRID 1394358
ノート
印刷プレビュー

反応式

HRID 1394358 の反応式
C(O[C:6]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][N:15]2[CH:19]=[N:18][CH:17]=[N:16]2)[CH2:10][CH2:9]1)=O)(C)(C)C.[F:20][C:21]([F:26])([F:25])[C:22]([OH:24])=[O:23].[C:27]([N:30]1[CH2:35][CH2:34][CH:33]([C:36]([N:38]([C:43]2[CH:48]=[CH:47][CH:46]=[C:45]([Cl:49])[CH:44]=2)[CH2:39][CH2:40]CCl)=[O:37])[CH2:32][CH2:31]1)(=[O:29])[CH3:28].C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[Cl-].[Na+]>ClCCl.O>[F:20][C:21]([F:26])([F:25])[C:22]([OH:24])=[O:23].[C:27]([N:30]1[CH2:35][CH2:34][CH:33]([C:36]([N:38]([C:43]2[CH:48]=[CH:47][CH:46]=[C:45]([Cl:49])[CH:44]=2)[CH2:39][CH2:40][CH2:6][N:8]2[CH2:9][CH2:10][CH:11]([CH2:14][N:15]3[CH:19]=[N:18][CH:17]=[N:16]3)[CH2:12][CH2:13]2)=[O:37])[CH2:32][CH2:31]1)(=[O:29])[CH3:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 4875Potassium IodideHCID 5234Sodium ChlorideHCID 6422Trifluoroacetic acidHCID 11430Potassium CarbonateHCID 18538476HCID 18538476、化合物HCID 18538822HCID 18538822、化合物

生成物 1

HCID 18538984
HCID 18538984、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-tert-butoxycarbonyl-4-(1H-1,2,4-triazol-1-ylmethyl)piperidine (48 mg, 0.18 mmol) in dry dichloromethane (1.5 mL) was added trifluoroacetic acid (1.5 mL), and the mixture was stirred at room temperature for 30 minutes. The solvent was distilled of under reduced pressure, and the residue was dissolved in methanol (1 mL). The solvent was distilled off under reduced pressure, and the residue 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 water. The mixture was saturated with sodium chloride, and 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 (49.1 mg, 58%).

後処理

  1. distillationThe solvent was distilled of under reduced pressure
  2. dissolutionthe residue was dissolved in methanol (1 mL)
  3. distillationThe solvent was distilled off under reduced pressure
  4. dissolutionthe residue was dissolved in dry acetonitrile (1.5 mL)
  5. stirringthe mixture was stirred at 80° C. for 5 hours
  6. temperatureThe mixture was cooled to room temperature
  7. extractionextracted three times with ethyl acetate (2 mL)
  8. concentrationconcentrated under reduced pressure
  9. customThe concentrate was purified

出典と根拠

ORDレコード
ord-c115f97b82a74e60a1241f71bde1cd92
出典データセット
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07348324B2

反応ノート

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