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Ammonia → Jnj-49095397

HRID 2067003
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HRID 2067003 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([CH2:8][O:9][C:10]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[C:13]([NH:20][C:21]([NH:23][C:24]3[N:28]([C:29]4[CH:34]=[CH:33][C:32]([CH3:35])=[CH:31][CH:30]=4)[N:27]=[C:26]([C:36]([CH3:39])([CH3:38])[CH3:37])[CH:25]=3)=[O:22])=[CH:12][CH:11]=2)[CH:5]=[CH:4][N:3]=1.CCN(C(C)C)C(C)C.[CH3:49][O:50][CH2:51][C:52](Cl)=[O:53].N>CO.CN(C=O)C.C(Cl)Cl>[C:36]([C:26]1[CH:25]=[C:24]([NH:23][C:21](=[O:22])[NH:20][C:13]2[C:14]3[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:10]([O:9][CH2:8][C:6]3[CH:5]=[CH:4][N:3]=[C:2]([NH:1][C:52](=[O:53])[CH2:51][O:50][CH3:49])[CH:7]=3)=[CH:11][CH:12]=2)[N:28]([C:29]2[CH:30]=[CH:31][C:32]([CH3:35])=[CH:33][CH:34]=2)[N:27]=1)([CH3:39])([CH3:38])[CH3:37]
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참가 물질

8

반응물 4

HCID 222AmmoniaHCID 81531Diisopropylethylamine2회HCID 96623Methoxyacetyl chloride2회HCID 584167531-(4-((2-Aminopyridin-4-yl)methoxy)naphthalen-1-yl)-3-(3-tert-butyl-1-p-tolyl-1H-pyrazol-5-yl)urea

생성물 1

HCID 45109868Jnj-49095397수율 50.3%

시약·촉매·용매 3

HCID 887
Methanol
용매
HCID 6228Dimethylformamide용매
HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 1-{4-[(2-aminopyridin-4-yl)methoxy]naphthalen-1-yl}-3-(3-tert-butyl-1-p-tolyl-1H-pyrazol-5-yl)urea (5) (526 mg, 0.96 mmol) and DIPEA (184 μL, 1.06 mmol) in mixture of DCM and DMF (10:1, 11 mL) was added methoxyacetyl chloride (92 μL, 1.01 mmol). After 1 h at RT further aliquots, of DIPEA (184 μL, 1.06 mmol) and methoxyacetyl chloride (92 μL, 1.01 mmol) were added sequentially and stirring was continued for 1 h. A solution of 1% ammonia in MeOH (40 mL), was added and the mixture stirred for 15 mins and then concentrated in vacuo. The crude product was purified by flash column chromatography (Biotage 40 g); eluting with 0 to 6% MeOH in DCM to furnish N-[4-({4-[3-(3-tert-butyl-1-p-tolyl-1H-pyrazol-5-yl)ureido]naphthalen-1-yloxy}methyl)pyridin-2-yl]-2-methoxyacetamide (1) (286 mg, 49%): m/z 593 (M+H)+ (ES+). 1H NMR (400 MHz, DMSO-d6) δ: 1.27 (9H, s), 2.39 (3H, s), 3.32 (3H, s), 4.08 (2H, s), 5.39 (2H, s), 6.36 (1H, s), 7.03 (1H, d), 7.28 (1H, dd), 7.36 (2H, m), 7.44 (2H, m), 7.56-7.64 (3H, m), 7.93 (1H, m), 8.30-8.35 (3H, m), 8.58 (1H, s), 8.79 (1H, s) and 10.02 (1H, s).

후처리

  1. waitwas continued for 1 h
  2. stirringthe mixture stirred for 15 mins
  3. concentrationconcentrated in vacuo
  4. customThe crude product was purified by flash column chromatography (Biotage 40 g)
  5. washeluting with 0 to 6% MeOH in DCM

출처 및 근거

ORD 기록
ord-598f3b52969948509c22aee23b761101
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08293771B2

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