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Hydrochloric Acid → 3-Methyl-5-(5-(4-(5-methylfuran-2-yl)phenyl)-8-oxo-6-thioxo-5,7-diazaspiro[3.4]octan-7-yl)picolinonitrile

HRID 515811
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HRID 515811 반응식
[C:1](Cl)(Cl)=[S:2].[CH3:5][C:6]1[O:10][C:9]([C:11]2[CH:16]=[CH:15][C:14]([NH:17][C:18]3([C:22]#[N:23])[CH2:21][CH2:20][CH2:19]3)=[CH:13][CH:12]=2)=[CH:8][CH:7]=1.N[C:25]1[CH:26]=[C:27]([CH3:33])[C:28]([C:31]#[N:32])=[N:29][CH:30]=1.Cl.CC(N(C)C)=[O:37]>O.CO>[CH3:33][C:27]1[C:28]([C:31]#[N:32])=[N:29][CH:30]=[C:25]([N:23]2[C:22](=[O:37])[C:18]3([CH2:21][CH2:20][CH2:19]3)[N:17]([C:14]3[CH:15]=[CH:16][C:11]([C:9]4[O:10][C:6]([CH3:5])=[CH:7][CH:8]=4)=[CH:12][CH:13]=3)[C:1]2=[S:2])[CH:26]=1
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참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 10040ThiophosgeneHCID 31374DimethylacetamideHCID 218645665-Amino-3-methylpyridine-2-carbonitrile2회HCID 673735051-((4-(5-Methylfuran-2-yl)phenyl)amino)cyclobutanecarbonitrile2회

생성물 1

HCID 53373213
3-Methyl-5-(5-(4-(5-methylfuran-2-yl)phenyl)-8-oxo-6-thioxo-5,7-diazaspiro[3.4]octan-7-yl)picolinonitrile

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
60 °C

실험 절차

Thiophosgene (0.1 mL) was added dropwise to a solution of 1-((4-(5-methylfuran-2-yl)phenyl)amino)cyclobutanecarbonitrile (Intermediate 106, 280 mg, 1.11 mmol) and 5-amino-3-methylpicolinonitrile (Intermediate 2, 177 mg, 1.33 mmol) in DMA (20 mL). The resulting mixture was stirred at 60° C. overnight. MeOH (16 mL) and HCl (2M, 8 mL) were added and the mixture was refluxed for 2 h then cooled to room temperature. The reaction mixture was poured into water (200 mL) and extracted with EtOAc. The organic layer was washed with brine, dried over Sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel (1:3 EtOAc/petroleum ether), to afford 140 mg of 3-methyl-5-(5-(4-(5-methylfuran-2-yl)phenyl)-8-oxo-6-thioxo-5,7-diazaspiro[3.4]octan-7-yl)picolinonitrile. 1H NMR (400 MHz, DMSO-d6) δ 8.74 (s, 1H), 8.16 (s, 1H), 7.86 (d, 2H), 7.46 (d, 2H), 6.98 (d, 1H), 6.28 (d, 1H), 2.63 (m, 2H), 2.60 (s, 3H), 2.51-2.43 (m, 2H), 2.38 (s, 3H), 1.97 (m, 1H), 1.57 (m, 1H). LCMS [M+1]+ 429.1.

후처리

  1. temperaturethe mixture was refluxed for 2 h
  2. temperaturethen cooled to room temperature
  3. extractionextracted with EtOAc
  4. washThe organic layer was washed with brine
  5. dry with materialdried over Sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography on silica gel (1:3 EtOAc/petroleum ether)

출처 및 근거

ORD 기록
ord-f4b932e25d2d444fa6ebb48326a2584e
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09108944B2

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