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Benzophenone imine → 4-[(4-Acetylpiperazin-1-yl)methyl]-2-amino-3-fluoropyridine

HRID 1355532
ノート
印刷プレビュー

反応式

HRID 1355532 の反応式
Cl[C:2]1[C:7]([F:8])=[C:6]([CH2:9][N:10]2[CH2:15][CH2:14][N:13]([C:16](=[O:18])[CH3:17])[CH2:12][CH2:11]2)[CH:5]=[CH:4][N:3]=1.CC([O-])(C)C.[Na+].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.C(=[NH:84])(C1C=CC=CC=1)C1C=CC=CC=1.Cl.C1COCC1>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:16]([N:13]1[CH2:14][CH2:15][N:10]([CH2:9][C:6]2[CH:5]=[CH:4][N:3]=[C:2]([NH2:84])[C:7]=2[F:8])[CH2:11][CH2:12]1)(=[O:18])[CH3:17]
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 5

HCID 136809Benzophenone imineHCID 634876Binap, (A+-)-HCID 18422008HCl tetrahydrofuranHCID 185069231-[4-(2-Chloro-3-fluoro-pyridin-4-ylmethyl)-piperazin-1-yl]-ethanoneHCID 23676156Sodium t-butoxide

生成物 1

HCID 185068144-[(4-Acetylpiperazin-1-yl)methyl]-2-amino-3-fluoropyridine

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

To a solution of 4-[(4-acetylpiperazin-1-yl)methyl]-2-chloro-3-fluoropyridine (14-3, 85 mg, 0.31 mmole) in dry toluene (2 mL) was added NaOtBu (42 mg, 0.44 mmole), racemic BINAP (29 mg, 0.05 mmole), Pd2(dba)3 (14 mg, 0.02 mmole), and benzophenone imine (0.06 mL, 0.38 mmole) then the mixture was heated to 80° C. After 18 hr the mixture was cooled to RT. A solution of 1N HCl:THF (1:1, 10 mL) was added and the mixture stirred for 1 hr. The mixture was washed with EtOAc (2×). The aqueous layer was made basic with saturated NaHCO3 then extracted with EtOAc (3×). The combined organic layers were dried (Na2SO4), filtered, and concentrated. Flash column chromatography (gradient, 0-5% MeOH/CH2Cl2) gave the titled compound as a light yellow solid: 1H-NMR (500 MHz, CDCl3) δ 7.81 (d, 1 H, J=5.12 Hz), 6.71 (t, 1 H, J=4.88 Hz), 4.56 (bs, 2 H), 3.63 (t, 2 H, J=5.13 Hz), 3.56 (s, 2 H), 3.10 (t, 2 H, J=5.13 Hz), 2.46 (m, 2 H), 2.08 (s, 3 H); MS (ES) (M+H)+ 253.

後処理

  1. temperatureAfter 18 hr the mixture was cooled to RT
  2. washThe mixture was washed with EtOAc (2×)
  3. extractionthen extracted with EtOAc (3×)
  4. dry with materialThe combined organic layers were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-b388004f05be4e1b84ef12675ddb6ff9
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06586424B2

反応ノート

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