Isopropyl iodide → 1-Isopropyl-4-(1-(4-fluorophenyl)-2-{4-[4-(2-methoxynaphthalen-1-yl)butyl]piperazin-1-yl}-2-oxoethyl)piperidine

HRID 497348ノート

反応式

HRID 497348 の反応式
Cl.[F:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([CH:34]2[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]2)[C:10]([N:12]2[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][CH2:20][CH2:21][C:22]3[C:31]4[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=4)[CH:25]=[CH:24][C:23]=3[O:32][CH3:33])[CH2:14][CH2:13]2)=[O:11])=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].I[CH:47]([CH3:49])[CH3:48]>CN(C)C=O.C(OCC)(=O)C>[CH:47]([N:37]1[CH2:36][CH2:35][CH:34]([CH:9]([C:6]2[CH:7]=[CH:8][C:3]([F:2])=[CH:4][CH:5]=2)[C:10]([N:12]2[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][CH2:20][CH2:21][C:22]3[C:31]4[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=4)[CH:25]=[CH:24][C:23]=3[O:32][CH3:33])[CH2:14][CH2:13]2)=[O:11])[CH2:39][CH2:38]1)([CH3:49])[CH3:48]

参加物

6

反応物 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 223186734-(1-(4-Fluorophenyl)-2-{4-[4-(2-methoxynaphthalen-1-yl)butyl]piperazin-1-yl}-2-oxoethyl)piperidine hydrochloride

生成物 1

HCID 223186581-Isopropyl-4-(1-(4-fluorophenyl)-2-{4-[4-(2-methoxynaphthalen-1-yl)butyl]piperazin-1-yl}-2-oxoethyl)piperidine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

0.20 g of 4-(1-(4-Fluorophenyl)-2-{4-[4-(2-methoxynaphthalen-1-yl)butyl]piperazin-1-yl}-2-oxoethyl)piperidine hydrochloride obtained in Example 11(5) was dissolved in 2 ml of dimethylformamide, and 93 mg of potassium carbonate and 41 μl of 2-iodopropane were added, followed by stirring at room temperature overnight. The reaction solution was diluted with ethyl acetate and washed with a saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous sodium sulfate. After removal of the drying agent by filtration, the filtrate was concentrated under reduced pressure. The residue was purified by a silica gel column chromatography (Chromatorex NH, hexane:ethyl acetate=4:1) to give 0.15 g of 1-isopropyl-4-(1-(4-fluorophenyl)-2-{4-[4-(2-methoxynaphthalen-1-yl)butyl]piperazin-1-yl}-2-oxoethyl)piperidine as an oil.

後処理

  1. washwashed with a saturated aqueous sodium bicarbonate solution
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customAfter removal of the drying agent
  4. filtrationby filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe residue was purified by a silica gel column chromatography (Chromatorex NH, hexane:ethyl acetate=4:1)

出典と根拠

ORDレコード
ord-2bdf79c0f23242aab685c7d066100749
出典データセット
uspto-grants-2005_09
特許番号
US06949552B2

反応ノート

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