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Triethylamine → 4-(2,2-Dimethyl-propylamino)-5-[3-(4-pyridin-2-yl-piperazin-1-yl)-prop-1-ynyl]-pyrimidine-2-carbonitrile

HRID 1163014
ノート
印刷プレビュー

反応式

HRID 1163014 の反応式
[CH2:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=2)[CH2:6][CH2:5]1)[C:2]#[CH:3].Br[C:17]1[C:18]([NH:25][CH2:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[N:19][C:20]([C:23]#[N:24])=[N:21][CH:22]=1.C(N(CC)CC)C>CN(C=O)C.O.[Cu]I.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH3:28][C:27]([CH3:30])([CH3:29])[CH2:26][NH:25][C:18]1[C:17]([C:3]#[C:2][CH2:1][N:4]2[CH2:9][CH2:8][N:7]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=3)[CH2:6][CH2:5]2)=[CH:22][N:21]=[C:20]([C:23]#[N:24])[N:19]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 8471TriethylamineHCID 106319131-(2-Propynyl)-4-(2-pyridinyl)-piperazineHCID 179681615-Bromo-4-(2,2-dimethylpropylamino)pyrimidine-2-carbonitrile

生成物 1

HCID 117410624-(2,2-Dimethyl-propylamino)-5-[3-(4-pyridin-2-yl-piperazin-1-yl)-prop-1-ynyl]-pyrimidine-2-carbonitrile収率 97%

試薬・触媒・溶媒 4

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 178418476HCID 178418476、化合物触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

1-(2-Propynyl)-4-(2-pyridinyl)-piperazine (prepared from 1-(2-pyridinyl)-piperazine and propargyl bromide) (1.5 mmol) is dissolved in DMF at room temperature under nitrogen atmosphere. To the solution, 5-bromo-4-(2,2-dimethyl-propylamino)-pyrimidine-2-carbonitrile (1 mmol), triethylamine (3 mmol), copper(I) iodide (0.1 mmol), and dichlorobis(triphenylphosphine)palladium(II) (0.05 mmol) are added successively. The mixture is heated at 80° C. under nitrogen atmosphere for 3 h. After cooling at room temperature, the mixture is diluted with H2O and extracted with AcOEt. The organic layer is dried over magnesium sulfate and evaporated in vacuo. The residue is purified by silica gel column chromatography (n-hexane:AcOEt=1:5) to give 4-(2,2-dimethyl-propylamino)-5-[3-(4-pyridin-2-yl-piperazin-1-yl)-prop-1-ynyl]-pyrimidine-2-carbonitrile. Yield 97%. Rf=0.30 (n-hexane:AcOEt 1:5). 1H NMR (400 MHz, CDCl3) δ 0.95 (s, 9H), 2.75-2.73 (m, 4H), 3.36 (d, 2H), 3.63-3.60 (m, 4H), 3.69 (s, 2H), 5.78 (brs, 1H), 6.63-6.67 (m, 2H), 7.47-7.52 (m, 1H), 8.19-8.21 (m, 2H).

後処理

  1. temperatureAfter cooling at room temperature
  2. extractionextracted with AcOEt
  3. dry with materialThe organic layer is dried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue is purified by silica gel column chromatography (n-hexane:AcOEt=1:5)

出典と根拠

ORDレコード
ord-96fffc12757b4a53b5e1b8c874d8bb45
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820818B2

反応ノート

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