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1-(1-Ethylpiperazin-4-yl)-3-bromoisoquinoline → HCID 22503411, 화합물

HRID 1006977
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HRID 1006977 반응식
[CH2:1]([O:8][CH2:9][CH2:10][NH:11][C:12](=[O:32])[C:13]1[CH:18]=[CH:17][C:16]([Sn](CCCC)(CCCC)CCCC)=[CH:15][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:34]1[N:35]=[C:36]([N:44]2[CH2:49][CH2:48][N:47]([CH2:50][CH3:51])[CH2:46][CH2:45]2)[C:37]2[C:42]([CH:43]=1)=[CH:41][CH:40]=[CH:39][CH:38]=2>C1(C)C(C)=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:50]([N:47]1[CH2:46][CH2:45][N:44]([C:36]2[C:37]3[C:42](=[CH:41][CH:40]=[CH:39][CH:38]=3)[CH:43]=[C:34]([C:16]3[CH:15]=[CH:14][C:13]([C:12](=[O:32])[NH:11][CH2:10][CH2:9][O:8][CH2:1][C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=4)=[CH:18][CH:17]=3)[N:35]=2)[CH2:49][CH2:48]1)[CH3:51]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 225024471-(1-Ethylpiperazin-4-yl)-3-bromoisoquinolineHCID 22503540HCID 22503540, 화합물

생성물 1

HCID 22503411HCID 22503411, 화합물수율 22.5%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 7237O-Xylene용매

실험 절차

N-(2-Benzyloxyethyl)-4-tributylstannylbenzamide (1.23 g) and 3-bromo-1-(4-ethylpiperazin-1-yl)isoquinoline (0.49 g) were heated under reflux in the presence of tetrakistriphenylphosphinepalladium(0) (0.13 g) in xylene in nitrogen atmosphere for 3 hr. After cooling, the reaction solution was filtered and concentrated. The resulting residue was purified by silica gel column chromatography (chloroform/methanol system). The resulting product was dissolved in ethyl acetate and extracted with 2N hydrochloric acid. The aqueous layer was washed with ethyl acetate, adjusted to pH 10 with a 8N aqueous solution of sodium hydroxide, and then extracted with ethyl acetate. The extract was washed with a 10% aqueous solution of sodium carbonate and brine, and dried over magnesium sulfate. The solvent was evaporated, to give 1-(4-ethylpiperazin-1-yl)-3-{4-[N-(2-benzyloxyethyl)carbamoyl]phenyl}isoquinoline (0.17 g) as a pale brown viscous oil.

후처리

  1. temperatureAfter cooling
  2. filtrationthe reaction solution was filtered
  3. concentrationconcentrated
  4. customThe resulting residue was purified by silica gel column chromatography (chloroform/methanol system)
  5. dissolutionThe resulting product was dissolved in ethyl acetate
  6. extractionextracted with 2N hydrochloric acid
  7. washThe aqueous layer was washed with ethyl acetate
  8. extractionextracted with ethyl acetate
  9. washThe extract was washed with a 10% aqueous solution of sodium carbonate and brine
  10. dry with materialdried over magnesium sulfate
  11. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-610755ac53dc40228b09f3a96e96eb95
출처 데이터셋
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06790844B2

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