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Cycloheptylamine → 6-chloro-N2-(3-chloro-4-methoxy-phenyl)-N4-cycloheptyl-pyrimidine-2,4-diamine

HRID 1161655
ノート
印刷プレビュー

反応式

HRID 1161655 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:10][C:11]2[N:16]=[C:15](Cl)[CH:14]=[C:13]([Cl:18])[N:12]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[CH:19]1([NH2:26])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.C(N(CC)CC)C>C(O)CCC>[Cl:18][C:13]1[N:12]=[C:11]([NH:10][C:4]2[CH:5]=[CH:6][C:7]([O:8][CH3:9])=[C:2]([Cl:1])[CH:3]=2)[N:16]=[C:15]([NH:26][CH:19]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]2)[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 2899CycloheptylamineHCID 8471TriethylamineHCID 58626087(3-Chloro-4-methoxy-phenyl)-(4,6-dichloro-pyrimidin-2-yl)-amine

生成物 1

HCID 586260766-chloro-N2-(3-chloro-4-methoxy-phenyl)-N4-cycloheptyl-pyrimidine-2,4-diamine収率 60%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

To a solution of compound (3-chloro-4-methoxy-phenyl)-(4,6-dichloro-pyrimidin-2-yl)-amine (0.08 g, 0.26 mmol) in butanol (3 mL) was added to cycloheptylamine (0.03 g, 0.26 mmol) at 25° C. with stirring. To this was added triethylamine (0.14 mL, 1.04 mmol), and the mixture was stirred for 30 minutes at 25° C. and then heated and refluxed for 12 hours under nitrogen atmosphere. The mixture was concentrated under vacuum, diluted with cold water, and extracted with ethyl acetate. The organic layers were collected, combined, washed with brine, dried over anhydrous sodium sulphate, and concentrated under vacuum to give the desired compound. Yield: 60%.

後処理

  1. stirringthe mixture was stirred for 30 minutes at 25° C.
  2. temperatureheated
  3. temperaturerefluxed for 12 hours under nitrogen atmosphere
  4. concentrationThe mixture was concentrated under vacuum
  5. additiondiluted with cold water
  6. extractionextracted with ethyl acetate
  7. customThe organic layers were collected
  8. washwashed with brine
  9. dry with materialdried over anhydrous sodium sulphate
  10. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-6e5260e4ff7e44e7abdb032391bb80f7
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820654B2

反応ノート

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