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Sodium Hydroxide → N-(3-Iodo-4-methyl-phenyl)-6-[4-(4-methoxy-phenyl)-piperazin-1-yl]-nicotinamide

HRID 2190635
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HRID 2190635 반응식
Cl.Cl.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1.[OH-].[Na+].C(N(C(C)C)CC)(C)C.Cl[C:29]1[CH:45]=[CH:44][C:32]([C:33]([NH:35][C:36]2[CH:41]=[CH:40][C:39]([CH3:42])=[C:38]([I:43])[CH:37]=2)=[O:34])=[CH:31][N:30]=1.Cl.COC1C=CC(N2CCNCC2)=CC=1>CN(C1C=CN=CC=1)C.C(Cl)Cl>[I:43][C:38]1[CH:37]=[C:36]([NH:35][C:33](=[O:34])[C:32]2[CH:44]=[CH:45][C:29]([N:14]3[CH2:15][CH2:16][N:11]([C:8]4[CH:7]=[CH:6][C:5]([O:4][CH3:3])=[CH:10][CH:9]=4)[CH2:12][CH2:13]3)=[N:30][CH:31]=2)[CH:41]=[CH:40][C:39]=1[CH3:42]
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참가 물질

8

반응물 5

HCID 14798Sodium HydroxideHCID 81531Diisopropylethylamine2회HCID 27237001-(4-Methoxyphenyl)-piperazine, dihydrochlorideHCID 79255626-chloro-N-(3-iodo-4-methyl-phenyl)-nicotinamideHCID 122011971-(4-Methoxyphenyl)piperazine hydrochloride

생성물 1

HCID 59318182
N-(3-Iodo-4-methyl-phenyl)-6-[4-(4-methoxy-phenyl)-piperazin-1-yl]-nicotinamide

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

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온도
120 °C

실험 절차

4-methoxyphenyl piperazine dihydrochloride (110 mg, 0.41 mmol) was partitioned between CH2Cl2 and 2N aq. NaOH. The aqueous layer was extracted twice more with CH2Cl2 and the combined organic layer was dried and concentrated. The residue was dissolved in dioxane (6 mL). The solution was then treated with diisopropyl ethylamine (0.07 mL, 0.41 mmol), a catalytic amount of DMAP and 6-chloro-N-(3-iodo-4-methyl-phenyl)-nicotinamide (50 mg, 0.13 mmol). The mixture was heated in a sealed tube at 120° C. for 22 hr. The mixture was then cooled, followed addition of another portion of 4-methoxyphenyl piperazine hydrochloride (110 mg, 0.41 mmol) and diisopropyl ethyl amine (0.14 mL, 0.82 mmol). The mixture was stirred at 120° C. for 3 more days then cooled and partitioned between EtOAc and aq. saturated Na2CO3. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was chromatographed on a silica gel column with 20-40% EtOAc in hexanes to afford the product. HRMS m/z calcd for C24H25N4O2I [M+H]+: 529.1095. Found: 529.1098.

후처리

  1. extractionThe aqueous layer was extracted twice more with CH2Cl2
  2. customthe combined organic layer was dried
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved in dioxane (6 mL)
  5. temperatureThe mixture was then cooled
  6. temperaturethen cooled
  7. custompartitioned between EtOAc and aq. saturated Na2CO3
  8. dry with materialThe organic layer was dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe residue was chromatographed on a silica gel column with 20-40% EtOAc in hexanes
  12. customto afford the product

출처 및 근거

ORD 기록
ord-0e384de5a2e243248fa4d140a5a3d237
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08324385B2

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