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

HRID 384684
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HRID 384684 반응식
[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
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참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
90 °C

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-7df4f2406c0748599f82104f3a00b672
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367658B2

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