Hydrochloric Acid → 2-{[5-Fluoro-2-({3-[2-(4-morpholinyl)ethyl]phenyl}amino)-4-pyrimidinyl]amino}-N-(2-hydroxyethyl)benzamide

HRID 1362870ノート

反応式

HRID 1362870 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:20]=[CH:19][CH:18]=[CH:17][C:10]=2[C:11]([NH:13][CH2:14][CH2:15][OH:16])=[O:12])[C:5]([F:21])=[CH:4][N:3]=1.[O:22]1[CH2:27][CH2:26][N:25]([CH2:28][CH2:29][C:30]2[CH:31]=[C:32]([CH:34]=[CH:35][CH:36]=2)[NH2:33])[CH2:24][CH2:23]1.Cl>C(O)(C)C>[F:21][C:5]1[C:6]([NH:8][C:9]2[CH:20]=[CH:19][CH:18]=[CH:17][C:10]=2[C:11]([NH:13][CH2:14][CH2:15][OH:16])=[O:12])=[N:7][C:2]([NH:33][C:32]2[CH:34]=[CH:35][CH:36]=[C:30]([CH2:29][CH2:28][N:25]3[CH2:24][CH2:23][O:22][CH2:27][CH2:26]3)[CH:31]=2)=[N:3][CH:4]=1

参加物

5

反応物 3

HCID 313Hydrochloric Acid2 回HCID 230715613-(Morpholinoethyl)anilineHCID 579741542-[(2-Chloro-5-fluoro-4-pyrimidinyl)amino]-N-(2-hydroxyethyl)benzamide

生成物 1

HCID 509437342-{[5-Fluoro-2-({3-[2-(4-morpholinyl)ethyl]phenyl}amino)-4-pyrimidinyl]amino}-N-(2-hydroxyethyl)benzamide収率 71.1%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
90 °C

実験手順

2-[(2-Chloro-5-fluoro-4-pyrimidinyl)amino]-N-(2-hydroxyethyl)benzamide (500 mg, 1.61 mmol) and 3-(morpholinoethyl)aniline (352 mg, 1.61 mmol) were combined in a tube with 30 mL isopropanol and 12N HCl (134 μL, 1.60 mmol). The vessel was sealed and heated with stirring at 90° C. for 18 h. The reaction was cooled to room temperature and the solid was filtered off and washed with isopropanol and ether to give 550 mg (71% yield) of a white solid as the HCl salt, LC/MS (M+H)+ 480, 481.

後処理

  1. customThe vessel was sealed
  2. temperatureheated
  3. temperatureThe reaction was cooled to room temperature
  4. filtrationthe solid was filtered off
  5. washwashed with isopropanol and ether

出典と根拠

ORDレコード
ord-4bc1018ddf6b48b5ae08d1888b9ef913
出典データセット
uspto-grants-2011_02
特許番号
US07884098B2

反応ノート

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