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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
ノート
印刷プレビュー

反応式

HRID 515811 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 10040ThiophosgeneHCID 31374DimethylacetamideHCID 218645665-Amino-3-methylpyridine-2-carbonitrile2 回HCID 673735051-((4-(5-Methylfuran-2-yl)phenyl)amino)cyclobutanecarbonitrile2 回

生成物 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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-f4b932e25d2d444fa6ebb48326a2584e
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09108944B2

反応ノート

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