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Hydrochloric Acid → 6-(4-Fluorophenyl)-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-ylamino)phenyl]pyrimidine-2,4-diamine

HRID 2240261
ノート
印刷プレビュー

反応式

HRID 2240261 の反応式
[F:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]2[N:16](COCC[Si](C)(C)C)[CH:17]=[CH:18][C:11]=12.Cl[C:28]1[CH:33]=[C:32]([C:34]2[CH:39]=[CH:38][C:37]([F:40])=[CH:36][CH:35]=2)[N:31]=[C:30]([NH2:41])[N:29]=1.Cl.[OH-].[Na+]>O>[F:40][C:37]1[CH:36]=[CH:35][C:34]([C:32]2[N:31]=[C:30]([NH2:41])[N:29]=[C:28]([NH:8][C:6]3[CH:5]=[CH:4][C:3]([NH:9][C:10]4[CH:15]=[CH:14][N:13]=[C:12]5[NH:16][CH:17]=[CH:18][C:11]=45)=[C:2]([F:1])[CH:7]=3)[CH:33]=2)=[CH:39][CH:38]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 14798Sodium HydroxideHCID 112183534-Chloro-6-(4-fluorophenyl)pyrimidin-2-amineHCID 593049942-Fluoro-N-(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)benzene-1,4-diamine

生成物 1

HCID 593049756-(4-Fluorophenyl)-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-ylamino)phenyl]pyrimidine-2,4-diamine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

100 mg (0.27 mmol) of 2-fluoro-N1-(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)benzene-1,4-diamine and 63 mg (0.28 mmol) of 4-chloro-6-(4-fluorophenyl)pyrimidine-2-amine are suspended in 3 ml of water. 39 μl (0.40 mmol) of a 37% strength hydrochloric acid solution are then added, and the mixture is heated under reflux overnight. After addition of a further 39 μl (0.40 mmol) of a 37% strength hydrochloric acid solution, the mixture is again reacted under reflux overnight. Using 1N aqueous sodium hydroxide solution, the suspension is then adjusted to pH 10, resulting in the precipitation of crystals. The solid is filtered off, washed with a little water and then dissolved in DMSO and purified by preparative RP-HPLC.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux overnight
  3. customthe mixture is again reacted
  4. temperatureunder reflux overnight
  5. customresulting in the precipitation of crystals
  6. filtrationThe solid is filtered off
  7. washwashed with a little water
  8. dissolutiondissolved in DMSO
  9. custompurified by preparative RP-HPLC

出典と根拠

ORDレコード
ord-1602cf236aca4247a7989579182d4c3a
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07723347B2

反応ノート

読み込み中…

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