Hydrochloric Acid → 2-(3-Fluoro-4-methoxy-phenyl)-6-(4-methoxy-phenyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalene

HRID 532677ノート

反応式

HRID 532677 の反応式
[F:1][C:2]1[CH:3]=[C:4]([C:10]2[S:11][C:12]3[CH2:13][C:14]4[C:20]([C:21]5[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][CH:22]=5)=[N:19][N:18](COCC[Si](C)(C)C)[C:15]=4[C:16]=3[CH:17]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].Cl>CO>[F:1][C:2]1[CH:3]=[C:4]([C:10]2[S:11][C:12]3[CH2:13][C:14]4[C:20]([C:21]5[CH:22]=[CH:23][C:24]([O:27][CH3:28])=[CH:25][CH:26]=5)=[N:19][NH:18][C:15]=4[C:16]=3[CH:17]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 866992472-(3-Fluoro-4-methoxy-phenyl)-6-(4-methoxy-phenyl)-4-(2-trimethylsilanyl-ethoxymethyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalene

生成物 1

HCID 718152422-(3-Fluoro-4-methoxy-phenyl)-6-(4-methoxy-phenyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalene収率 76.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

2-(3-Fluoro-4-methoxy-phenyl)-6-(4-methoxy-phenyl)-4-(2-trimethylsilanyl-ethoxymethyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalene (0.43 g, 0.8 mmol) was dissolved in MeOH and treated with concentrated HCl (0.25 mL, 8 mmol). The reaction mixture was heated at 100° C. for 4 hr. The solution was cooled to room temperature and the resultant precipitate was filtered, washed with MeOH and concentrated under reduced pressure to provide the corresponding 2-(3-Fluoro-4-methoxy-phenyl)-6-(4-methoxy-phenyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalene (0.24 g, 0.61 mmol) as yellow solid in 76% yield.

後処理

  1. temperatureThe solution was cooled to room temperature
  2. filtrationthe resultant precipitate was filtered
  3. washwashed with MeOH
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-0e6160556e0e4cefba9d0f620ec9500c
出典データセット
uspto-grants-2014_10
特許番号
US08853207B2

反応ノート

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