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Diisopropylethylamine → HCID 22318660, 화합물

HRID 497330
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HRID 497330 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([N:16]2[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]2)[CH2:9][N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:4][CH:3]=1.C(N(C(C)C)C(C)C)C.[F:32][C:33]1[CH:46]=[CH:45][C:36]2[C:37]([CH2:40][CH2:41][CH2:42][CH2:43]Cl)=[N:38][O:39][C:35]=2[CH:34]=1>CN(C)C=O.C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([N:16]2[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]2)[CH2:9][N:10]2[CH2:15][CH2:14][N:13]([CH2:43][CH2:42][CH2:41][CH2:40][C:37]3[C:36]4[CH:45]=[CH:46][C:33]([F:32])=[CH:34][C:35]=4[O:39][N:38]=3)[CH2:12][CH2:11]2)=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 9991338HCID 9991338, 화합물HCID 10957750Piperazine, 1-[1-(4-fluorophenyl)-2-(1-piperazinyl)ethyl]-4-methyl-

생성물 1

HCID 22318660HCID 22318660, 화합물수율 36.6%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매
HCID 8857
Ethyl Acetate
용매

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온도
120 °C

실험 절차

0.37 g of 1-[2-(4-Fluorophenyl)-2-(4-methylpiperazino)ethyl]piperazine obtained in Example 2 (4) was dissolved in 4.0 ml of dimethylformamide, and 0.19 g of N-ethyldiisopropylamine and 0.31 g of 4-(6-fluoro-1,2-benzisoxazol-3-yl)butyl chloride were added, followed by stirring at 120° C. for 3 hours. The reaction solution was cooled to room temperature, diluted with ethyl acetate and washed with water 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=1:1) to give 0.22 g of 1-[2-(4-fluorophenyl)-2-(4-methylpiperazino)ethyl]-4-[4-(6-fluoro-1,2-benzisoxazol-3-yl)butyl]piperazine as an oil.

후처리

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

출처 및 근거

ORD 기록
ord-3f39e1eff92c45d691cd705a0067d5aa
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06949552B2

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