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2,3-Butanediol → 4-Chloro-6-[5-chloro-2-(2,2,2-trifluoro-ethoxy)-phenyl]-pyrimidin-2-ylamine

HRID 28607
ノート
印刷プレビュー

反応式

HRID 28607 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH2:12][C:13]([F:16])([F:15])[F:14])=[C:6](B(O)O)[CH:7]=1.[Cl:17][C:18]1[CH:23]=[C:22](Cl)[N:21]=[C:20]([NH2:25])[N:19]=1.CC(O)C(O)C.C(=O)([O-])[O-].[Na+].[Na+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[Cl:17][C:18]1[CH:23]=[C:22]([C:6]2[CH:7]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:11][CH2:12][C:13]([F:16])([F:15])[F:14])[N:21]=[C:20]([NH2:25])[N:19]=1
参加物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 2622,3-ButanediolHCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 655222-Amino-4,6-dichloropyrimidineHCID 689852805-Chloro-2-(2,2,2-trifluoro-ethoxy)-phenylboronic acid

生成物 1

HCID 860043624-Chloro-6-[5-chloro-2-(2,2,2-trifluoro-ethoxy)-phenyl]-pyrimidin-2-ylamine

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 962Water溶媒

実験手順

To a mixture of 5-chloro-2-(2,2,2-trifluoro-ethoxy)-phenylboronic acid (1.6 g, 6.3 mmol), 4,6-dichloro-pyrimidin-2-ylamine (1.2 g, 7.6 mmol), palladium acetate (211 mg, 0.95 mmol), and dimethyl ethylene glycol (100 ml), degassed with argon, was added a solution of sodium carbonate (4.0 g, 37.8 mmol) in water (15 ml) followed by triphenylphosphine (495 mg, 1.9 mmol). After stirring for 12 hours, the mixture was filtered through a pad of celite under suction. The organic layer was separated from the filtrate and dried over magnesium sulfate. The mixture was purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:5 followed by 1:4) to give 4-chloro-6-[5-chloro-2-(2,2,2-trifluoro-ethoxy)-phenyl]-pyrimidin-2-ylamine, which was dissolved in ethyl acetate (10 ml) and treated with a solution of hydrogen chloride in dioxane (4 M, 2.5 ml). The solid was filtered to provide the hydrochloride salt of 4-chloro-6-[5-chloro-2-(2,2,2-trifluoro-ethoxy)-phenyl]-pyrimidin-2-ylamine (500 mg, 20% yield). 1H NMR (CD3OD) δ 4.78 (q, 2H, J=8.5 Hz, CH2), 7.31-7.33 (m, 2H, Ar), 7.65 (dd, 1H, J=8.9 Hz, J=2.8 Hz, Ar), 7.82 (d, 1H, J=2.6 Hz, Ar).

後処理

  1. customdegassed with argon
  2. filtrationthe mixture was filtered through a pad of celite under suction
  3. customThe organic layer was separated from the filtrate
  4. dry with materialdried over magnesium sulfate
  5. customThe mixture was purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:5 followed by 1:4)

出典と根拠

ORDレコード
ord-5f52e4dd7ec94562be53befaa13e0729
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07419984B2

反応ノート

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