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Hydrochloric Acid → 3-(2-piperidin-4-yl-phenylsulfanyl)-1H-indole

HRID 2244047
ノート
印刷プレビュー

反応式

HRID 2244047 の反応式
Cl.C(OC([N:9]1[CH2:14][CH2:13][CH:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[S:21][C:22]2[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[NH:24][CH:23]=2)[CH2:11][CH2:10]1)=O)(C)(C)C.C([O-])(O)=O.[Na+]>C(OCC)C>[NH:9]1[CH2:14][CH2:13][CH:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[S:21][C:22]2[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[NH:24][CH:23]=2)[CH2:11][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 686342064-[2-(1H-indol-3-ylsulfanyl)-phenyl]-piperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 116952463-(2-piperidin-4-yl-phenylsulfanyl)-1H-indole

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

1.58 g 4-(2-Triisopropylsilanylsulfanyl-phenyl)-piperidine-1-carboxylic acid tert-butyl ester (3.51 mmol) in 10 mL THF was added to 1.21 g tetrabutylammonium fluoride dihydrate (3.85 mmol) in 5 mL THF at 0° C. The reaction mixture was stirred 1 hour at 0° C., filtered through a plug of silica (eluted with EtOAc/heptane 1:1) and concentrated in vacuo. The residue was redissolved in 14 mL THF. 2 mL of this solution (≈0.5 mmol) was added to 67 mg N-chloro succinimide (0.50 mmol) in 2 mL 1,2-dichloro-ethane at 0° C. The reaction mixture was stirred 30 minutes at room temperature. The resulting solution was added to 90 mg indole (0.75 mmol) in 2 mL THF at 0° C. The reaction mixture was stirred 2 hour at 0° C., poured into 20 mL saturated NaHCO3 and extracted with ethyl acetate (2×50 mL). The combined organic phases were washed with brine (20 mL), dried with MgSO4 and concentrated in vacuo. The residue was purified by flash chromatography (silica gel; ethyl acetate/heptane) to give 89 mg 4-[2-(1H-indol-3-ylsulfanyl)-phenyl]-piperidine-1-carboxylic acid tert-butyl ester (0.22 mmol, ≈44%). 2 mL diethyl ether saturated with HCl was added to 4-[2-(1H-indol-3-ylsulfanyl)-phenyl]-piperidine-1-carboxylic acid tert-butyl ester and stirred over night at room temperature. The reaction mixture was neutralized with saturated NaHCO3 and extracted with ethyl acetate (2×50 mL). The combined organic phases were washed with brine (20 mL), dried with MgSO4 and concentrated in vacuo. 3-(2-piperidin-4-yl-phenylsulfanyl)-1H-indole was isolated after preparative HPLC.

後処理

  1. extractionextracted with ethyl acetate (2×50 mL)
  2. washThe combined organic phases were washed with brine (20 mL)
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8f8bfab1fd144704890302dd9a1ceca8
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07678800B2

反応ノート

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