Hydrochloric Acid → 1-(2-Chloro-phenyl)-3-{6-[4-(3-morpholin-4-yl-propoxy)-phenylamino]-pyrimidin-4-yl}-urea

HRID 1038702ノート

反応式

HRID 1038702 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]([NH:11][C:12]1[CH:17]=[C:16](Cl)[N:15]=[CH:14][N:13]=1)=[O:10].[N:19]1([CH2:25][CH2:26][CH2:27][O:28][C:29]2[CH:34]=[CH:33][C:32]([NH2:35])=[CH:31][CH:30]=2)[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1.Cl>C(O)C.O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]([NH:11][C:12]1[CH:17]=[C:16]([NH:35][C:32]2[CH:33]=[CH:34][C:29]([O:28][CH2:27][CH2:26][CH2:25][N:19]3[CH2:20][CH2:21][O:22][CH2:23][CH2:24]3)=[CH:30][CH:31]=2)[N:15]=[CH:14][N:13]=1)=[O:10]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 220609034-(3-Morpholinopropoxy)anilineHCID 860869821-(2-Chloro-phenyl)-3-(6-chloro-pyrimidin-4-yl)-urea

生成物 1

HCID 577102331-(2-Chloro-phenyl)-3-{6-[4-(3-morpholin-4-yl-propoxy)-phenylamino]-pyrimidin-4-yl}-urea

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A solution of 1-(2-chloro-phenyl)-3-(6-chloro-pyrimidin-4-yl)-urea (99 mg, 0.35 mmol), 4-(3-morpholin-4-yl-propoxy)-phenylamine [Chabrier et al. Bull. Soc. Chim. Fr. 1955; 1353] (83 mg, 0.35 mmol), and concentrated HCl (0.1 ml, 1.4 mmol) in ethanol (5 ml) was refluxed for 32 h. The reaction mixture is cooled to RT, and diluted with water. The acidic solution is washed with ethyl acetate, basified with aqueous ammoniac, and extracted with DCM. The combined organic phases are dried over sodium sulfate, evaporated in vacuo, the residue is crystallized from water/methanol/1 N HCl to afford the title compound.

後処理

  1. washThe acidic solution is washed with ethyl acetate
  2. extractionextracted with DCM
  3. dry with materialThe combined organic phases are dried over sodium sulfate
  4. customevaporated in vacuo
  5. customthe residue is crystallized from water/methanol/1 N HCl

出典と根拠

ORDレコード
ord-e2cc3a53924d430daf9f9ea2783398f2
出典データセット
uspto-grants-2013_10
特許番号
US08552002B2

反応ノート

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