Hydrochloric Acid → [4-(4,7-Dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalen-6-yl)-phenyl]-(4-fluoro-phen yl)-amine

HRID 532545ノート

反応式

HRID 532545 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]3[C:19]4[CH2:20][C:21]5[S:22][CH:23]=[CH:24][C:25]=5[C:18]=4[N:17](COCC[Si](C)(C)C)[N:16]=3)=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.Cl>CO>[S:22]1[CH:23]=[CH:24][C:25]2[C:18]3[NH:17][N:16]=[C:15]([C:12]4[CH:11]=[CH:10][C:9]([NH:8][C:5]5[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=5)=[CH:14][CH:13]=4)[C:19]=3[CH2:20][C:21]1=2

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86699199(4-Fluoro-phenyl)-{4-[4-(2-trimethylsilanyl-ethoxymethyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalen-6-yl]-phenyl}-amine

生成物 1

HCID 71815875[4-(4,7-Dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalen-6-yl)-phenyl]-(4-fluoro-phen yl)-amine収率 85%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

(4-Fluoro-phenyl)-{4-[4-(2-trimethylsilanyl-ethoxymethyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalen-6-yl]-phenyl}-amine (0.25 g, 0.5 mmol) was dissolved in MeOH and treated with concentrated HCl (0.16 mL, 5 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 [4-(4,7-Dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalen-6-yl)-phenyl]-(4-fluoro-phen yl)-amine (0.14 g, 0.42 mmol) as white solid in 85% 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-94318b79311c405ea93eaeeeb4b4c792
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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