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Diisopropylethylamine → (4-Benzyl-6-methyl-pyrimidin-2-yl)-[1-(2-methyl-pyrimidin-4-yl)-piperidin-4-yl]-amine

HRID 451410
ノート
印刷プレビュー

反応式

HRID 451410 の反応式
Cl.Cl.[CH3:3][C:4]1[N:9]=[C:8]([N:10]2[CH2:15][CH2:14][CH:13]([NH2:16])[CH2:12][CH2:11]2)[CH:7]=[CH:6][N:5]=1.[CH2:17]([C:24]1[CH:29]=[C:28]([CH3:30])[N:27]=[C:26](Cl)[N:25]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(N(CC)C(C)C)(C)C>CN1CCCC1=O.O>[CH2:17]([C:24]1[CH:29]=[C:28]([CH3:30])[N:27]=[C:26]([NH:16][CH:13]2[CH2:14][CH2:15][N:10]([C:8]3[CH:7]=[CH:6][N:5]=[C:4]([CH3:3])[N:9]=3)[CH2:11][CH2:12]2)[N:25]=1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 81531DiisopropylethylamineHCID 673429791-(2-Methylpyrimidin-4-yl)piperidin-4-amine dihydrochlorideHCID 866336184-Benzyl-2-chloro-6-methyl-pyrimidine

生成物 1

HCID 53353336(4-Benzyl-6-methyl-pyrimidin-2-yl)-[1-(2-methyl-pyrimidin-4-yl)-piperidin-4-yl]-amine

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 13387
N-methyl-2-pyrrolidone
溶媒

実験手順

A solution of 1-(2-methyl-pyrimidin-4-yl)-piperidin-4-ylamine dihydrochloride (53 mg, 0.2 mmol), 4-benzyl-2-chloro-6-methylpyrimidin (48.1 mg, 0.22 mmol) and N,N-diisopropylethyl amine (120 L, 0.7 mmol) in N-methyl-pyrrolidinone (1 mL) was heated at 200° C. in a microwave oven for 1 hour. The reaction was diluted with water and extracted twice with ethyl acetate. The combined organic layers were washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel with AcOEt/EtOH 9:1 (v/v) as eluent. The title compound was obtained as a light yellow solid (16 mg, 21%).

後処理

  1. extractionextracted twice with ethyl acetate
  2. washThe combined organic layers were washed with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel with AcOEt/EtOH 9:1 (v/v) as eluent

出典と根拠

ORDレコード
ord-2cab62e0e16a4ee5a669efd938bde70e
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08486967B2

反応ノート

読み込み中…

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