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Ethanol → 7-(2-Chloro-6-fluorobenzyl)-1,3-dimethyl-8-phenyl-3,7-dihydro-1H-purine-2,6-dione

HRID 1727024
ノート
印刷プレビュー

反応式

HRID 1727024 の反応式
Br[C:2]1[N:10]([CH2:11][C:12]2[C:17]([F:18])=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:19])[C:9]2[C:8](=[O:20])[N:7]([CH3:21])[C:6](=[O:22])[N:5]([CH3:23])[C:4]=2[N:3]=1.C(O)C.[C:27]1(B(O)O)[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.[Cl-].[Li+]>C(=O)([O-])[O-].[Na+].[Na+].C1(C)C=CC=CC=1.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[Cl:19][C:13]1[CH:14]=[CH:15][CH:16]=[C:17]([F:18])[C:12]=1[CH2:11][N:10]1[C:9]2[C:8](=[O:20])[N:7]([CH3:21])[C:6](=[O:22])[N:5]([CH3:23])[C:4]=2[N:3]=[C:2]1[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=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

8

反応物 4

HCID 702EthanolHCID 66827Phenylboronic AcidHCID 433294Lithium ChlorideHCID 6592358-bromo-7-(2-chloro-6-fluorobenzyl)-1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione

生成物 1

HCID 117416077-(2-Chloro-6-fluorobenzyl)-1,3-dimethyl-8-phenyl-3,7-dihydro-1H-purine-2,6-dione収率 71.2%

試薬・触媒・溶媒 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 1140Toluene溶媒
HCID 10340Sodium Carbonate溶媒

反応条件

温度
100 °C

実験手順

A solution of 8-bromo-7-(2-chloro-6-fluorobenzyl)-1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione (100 mg, 0.25 mmol) in 260 μL aqueous sodium carbonate (2 M), 650 μL toluene, and 110 μL ethanol was treated with commercially available phenylboronic acid (34 mg, 0.27 mmol), tetrakis(triphenylphosphine)-palladium(0) (9 mg, 0.0075 mmol), and lithium chloride (catalytic). The reaction mixture was heated to 100° C. in a sealed vial and stirred overnight The reaction mixture was cooled and separated between water and ether. The aqueous layer was extracted with ether (3×) and the combined organics were dried with magnesium sulfate, filtered, and concentrated in vacuo. The crude product was purified by flash chromatography (silica gel cartridge, Biotage, 32-63 μm, 60 Å) with 50% EtOAc:hexanes as the eluent to afford 71 mg (71% yield) of the title compound as a white solid: 1H NMR (CDCl3, 300 MHz) 7.61-7.36 (m, 5H), 7.19-7.04 (m, 2H), 6.88-6.76 (m, 1H), 5.89 (s, 2H), 3.67 (s, 3H), 3.43 (s, 3H); MS (ESP+) m/e 400 (MH+); TLC (EtOAc:hexanes/1:1) Rf=0.45.

後処理

  1. temperaturewas cooled
  2. customseparated between water and ether
  3. extractionThe aqueous layer was extracted with ether (3×)
  4. dry with materialthe combined organics were dried with magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified by flash chromatography (silica gel cartridge, Biotage, 32-63 μm, 60 Å) with 50% EtOAc

出典と根拠

ORDレコード
ord-b76f314919c841328e813a22760887b2
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07495004B2

反応ノート

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