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Dimethylamine → (4-{[4-(4-Chlorophenyl)-pyrimidin-2-yl]amino}phenyl)-N,N-dimethyl carboxamide

HRID 1246766
ノート
印刷プレビュー

反応式

HRID 1246766 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]([NH:14][C:15]3[CH:23]=[CH:22][C:18]([C:19]([OH:21])=O)=[CH:17][CH:16]=3)[N:9]=2)=[CH:4][CH:3]=1.S(Cl)(Cl)=O.[CH3:28][NH:29][CH3:30].C(N(CC)CC)C>C1COCC1.O.CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]([NH:14][C:15]3[CH:23]=[CH:22][C:18]([C:19]([N:29]([CH3:30])[CH3:28])=[O:21])=[CH:17][CH:16]=3)[N:9]=2)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 674DimethylamineHCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 219060074-{[4-(4-Chlorophenyl)pyrimidin-2-yl]amino} benzoic acid

生成物 1

HCID 9975339(4-{[4-(4-Chlorophenyl)-pyrimidin-2-yl]amino}phenyl)-N,N-dimethyl carboxamide

試薬・触媒・溶媒 3

HCID 962Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 4-{[4-(4-chlorophenyl)pyrimidin-2-yl]amino}benzoic acid (200 mg, 0.615 mmol) is added thionyl chloride (4 mL) along with a catalytic amount of DMF at room temperature. The resulting suspension is then refluxed for a period of 1 hour resulting in a clear pale yellow solution which was concentrated in vacuo. To the flask was then added a solution of dimethylamine (615 μL of a 2.0 M solution in THF, 1.23 mmol) and triethylamine (124 mg, 1.23 mmol) in tetrahydrofuran (4.5 mL). The solution was then stirred for 18 hours at room temperature, diluted with water (5 mL) and filtered. Purification of the remaining solid by preparative HPLC yielded the title compound. HPLC/ES-MS: RT 6.74 min.(Method A); (m/z) 353 [M+1]+.

後処理

  1. temperatureThe resulting suspension is then refluxed for a period of 1 hour
  2. customresulting in a clear pale yellow solution which
  3. concentrationwas concentrated in vacuo
  4. filtrationfiltered
  5. customPurification of the remaining solid by preparative HPLC

出典と根拠

ORDレコード
ord-bfeb10b215e14d1884827e6cf19c063d
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07129242B2

反応ノート

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