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Potassium Phosphate, Tribasic → Methyl 6-(adamantan-1-ylmethoxy)-5-cyclopropylnicotinate

HRID 1427900
ノート
印刷プレビュー

反応式

HRID 1427900 の反応式
[C:1]12([CH2:11][O:12][C:13]3[C:22](Cl)=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][N:14]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.[CH:24]1(B(O)O)[CH2:26][CH2:25]1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].F[B-](F)(F)F.C1(P(C2CCCCC2)C2CCCCC2)CCCCC1>C1(C)C=CC=CC=1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[C:1]12([CH2:11][O:12][C:13]3[C:22]([CH:24]4[CH2:26][CH2:25]4)=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][N:14]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 2760897Cyclopropylboronic acidHCID 20066521Tri(cyclohexyl)phosphine tetrafluoroborateHCID 86702922Methyl 6-(adamantan-1-ylmethoxy)-5-chloronicotinate

生成物 1

HCID 86702923Methyl 6-(adamantan-1-ylmethoxy)-5-cyclopropylnicotinate収率 89.2%

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒
HCID 1140Toluene溶媒

実験手順

A mixture of methyl 6-(adamantan-1-ylmethoxy)-5-chloronicotinate (1.29 g, 3.84 mmol), cyclopropylboronic acid (0.43 g, 4.99 mmol), potassium phosphate (3.26 g, 15.40 mmol), tricyclohexylphosphine tetrafluoroborate (0.14 g, 0.38 mmol) and palladium acetate (0.04 g, 0.19 mmol) in degassed toluene (50 mL) and degassed water (5 mL) was refluxed under nitrogen for 7 h. The reaction mixture was cooled to ambient temperature and diluted with ethyl acetate (100 mL), washed with water (50 mL), saturated ammonium chloride (50 mL) and brine (50 mL); dried over anhydrous sodium sulfate, filtered through diatomaceous earth and concentrated in vacuo. The residue was purified by flash chromatography eluting with 5% ethyl acetate in hexanes to afford the title compound as a white solid (1.17 g, 89%); 1H NMR (300 MHz, CDCl3) δ 8.57 (d, J=2.2 Hz, 1H), 7.67 (d, J=2.2 Hz, 1H), 3.95 (s, 2H), 3.85 (s, 3H), 2.09-1.96 (m, 4H), 1.78-1.63 (m, 12H), 0.99-0.91 (m, 2H), 0.72-0.65 (m, 2H); MS (ES+) m/z: 342.22 (M+1).

後処理

  1. customdegassed water (5 mL)
  2. temperaturewas refluxed under nitrogen for 7 h
  3. additiondiluted with ethyl acetate (100 mL)
  4. washwashed with water (50 mL), saturated ammonium chloride (50 mL) and brine (50 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered through diatomaceous earth
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by flash chromatography
  9. washeluting with 5% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-4d039d9b3bf44f8587cd653f1bfc61d1
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08933236B2

反応ノート

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