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Methanol → N4-[3-Fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-ylmethyl)phenyl]-6-(trifluoromethyl)pyrimidine-2,4-diamine

HRID 2240264
ノート
印刷プレビュー

反応式

HRID 2240264 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[CH2:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]2[NH:16][CH:17]=[CH:18][C:11]=12)[NH2:5].Cl[C:20]1[CH:25]=[C:24]([C:26]([F:29])([F:28])[F:27])[N:23]=[C:22]([NH2:30])[N:21]=1.[OH-].[Na+].CO>O.Cl>[F:1][C:2]1[CH:3]=[C:4]([NH:5][C:20]2[CH:25]=[C:24]([C:26]([F:29])([F:27])[F:28])[N:23]=[C:22]([NH2:30])[N:21]=2)[CH:6]=[CH:7][C:8]=1[CH2:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]2[NH:16][CH:17]=[CH:18][C:11]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 130869074-Chloro-6-(trifluoromethyl)pyrimidin-2-amineHCID 593050333-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-ylmethyl)aniline

生成物 1

HCID 59305029N4-[3-Fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-ylmethyl)phenyl]-6-(trifluoromethyl)pyrimidine-2,4-diamine

試薬・触媒・溶媒 2

HCID 313
Hydrochloric Acid
溶媒
HCID 962Water溶媒

実験手順

32 mg (0.11 mmol) of 3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-ylmethyl)aniline and 26 mg (0.12 mmol) of 4-chloro-6-(trifluoromethyl)pyrimidine-2-amine are suspended in 5 ml of water and 0.07 ml of 2N hydrochloric acid. The reaction mixture is heated at reflux for 20 hours. After cooling, the mixture is made alkaline using dilute aqueous sodium hydroxide solution, a little methanol is added and the mixture is extracted with ethyl acetate. The extract is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by preparative HPLC.

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for 20 hours
  3. temperatureAfter cooling
  4. extractionthe mixture is extracted with ethyl acetate
  5. dry with materialThe extract is dried over sodium sulfate
  6. customthe solvent is removed under reduced pressure
  7. customThe residue is purified by preparative HPLC

出典と根拠

ORDレコード
ord-84a9ae195727482ba5a945629d9c773d
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

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