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Binap, (A+-)- → 5-(4-(1-Methylpiperidin-4-ylamino)-5-phenylpyridin-2-ylamino)pyrazine-2-carbonitrile

HRID 556845
ノート
印刷プレビュー

反応式

HRID 556845 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([NH:8][C:9]2[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:13][N:12]=[C:11]([NH2:21])[CH:10]=2)[CH2:4][CH2:3]1.Br[C:23]1[CH:28]=[N:27][C:26]([C:29]#[N:30])=[CH:25][N:24]=1.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1>[CH3:1][N:2]1[CH2:3][CH2:4][CH:5]([NH:8][C:9]2[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:13][N:12]=[C:11]([NH:21][C:23]3[N:24]=[CH:25][C:26]([C:29]#[N:30])=[N:27][CH:28]=3)[CH:10]=2)[CH2:6][CH2:7]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

6

反応物 4

HCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 378187222-Bromo-5-cyanopyrazineHCID 59613481N4-(1-Methylpiperidin-4-yl)-5-phenylpyridine-2,4-diamine

生成物 1

HCID 596134445-(4-(1-Methylpiperidin-4-ylamino)-5-phenylpyridin-2-ylamino)pyrazine-2-carbonitrile収率 17.3%

試薬・触媒・溶媒 1

HCID 1140
Toluene
溶媒

反応条件

温度
90 °C

実験手順

A solution of N4-(1-methylpiperidin-4-yl)-5-phenylpyridine-2,4-diamine (0.050 g, 0.17 mmol), 2-bromo-5-cyanopyrazine (0.022 g, 0.12 mmol), BINAP (0.003 g, 0.01 mmol), sodium tert-butoxide (0.016 g, 0.16 mmol), tris(dibenzylideneacetone)dipalladium chloroform complex (0.005 g, 0.01 mmol) in toluene (0.7 mL) was stirred at r.t. under nitrogen for 10 min before being heated under microwave irradiation for 30 min at 90° C. The crude reaction mixture was purified by ion exchange on SCX-II acidic resin (0.5 g) eluting with methanol/dichloromethane (1/1), then 2M ammonia-methanol. The basic fractions were combined and the solvent was removed in vacuo. The crude mixture was purified by preparative thin layer chromatography eluting with methanol/dichloromethane (1/9) to give the desired compound as a yellow solid (0.008 g, 17%).

後処理

  1. customThe crude reaction mixture
  2. customwas purified by ion exchange on SCX-II acidic resin (0.5 g)
  3. washeluting with methanol/dichloromethane (1/1)
  4. customthe solvent was removed in vacuo
  5. customThe crude mixture was purified by preparative thin layer chromatography
  6. washeluting with methanol/dichloromethane (1/9)

出典と根拠

ORDレコード
ord-c9e40f5975504d1c9860a7ee0abc46c2
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058045B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート