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Triethylamine → 1-[2-Chloro-6-(4-methoxy-benzylamino)-pyridin-4-ylmethyl]-6-(3-[1,3]dioxolan-2-yl-5-methyl-phenoxy)-5-isopropyl-1H-pyrimidine-2,4-dione

HRID 426214
ノート
印刷プレビュー

反応式

HRID 426214 の反応式
F[C:2]1[CH:7]=[C:6]([CH2:8]O)[CH:5]=[C:4]([NH:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)[N:3]=1.C(N(CC)CC)C.CS([Cl:31])(=O)=O.C([O:39][C:40]1[N:45]=[C:44]([O:46]CC2C=CC=CC=2)[C:43]([CH:54]([CH3:56])[CH3:55])=[C:42]([O:57][C:58]2[CH:63]=[C:62]([CH3:64])[CH:61]=[C:60]([CH:65]3[O:69][CH2:68][CH2:67][O:66]3)[CH:59]=2)[N:41]=1)C1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].[I-].[Li+]>C(Cl)(Cl)Cl.ClCCl.CN(C=O)C>[Cl:31][C:2]1[CH:7]=[C:6]([CH2:8][N:41]2[C:42]([O:57][C:58]3[CH:63]=[C:62]([CH3:64])[CH:61]=[C:60]([CH:65]4[O:69][CH2:68][CH2:67][O:66]4)[CH:59]=3)=[C:43]([CH:54]([CH3:56])[CH3:55])[C:44](=[O:46])[NH:45][C:40]2=[O:39])[CH:5]=[C:4]([NH:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 6

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 66321Lithium iodideHCID 59184650HCID 59184650、化合物HCID 591846532,4-Bis-benzyloxy-6-(3-[1,3]dioxolan-2-yl-5-methyl-phenoxy)-5-isopropyl-pyrimidine

生成物 1

HCID 59184794
1-[2-Chloro-6-(4-methoxy-benzylamino)-pyridin-4-ylmethyl]-6-(3-[1,3]dioxolan-2-yl-5-methyl-phenoxy)-5-isopropyl-1H-pyrimidine-2,4-dione
収率 57.2%

試薬・触媒・溶媒 3

HCID 6212Chloroform溶媒HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 2-fluoro-6-(p-methoxybenzylamino)-4-pyridine-methanol (790 mg, 2.84 mmol) in chloroform (28 ml) at 0° C. (ice bat), was added triethylamine (597 μl, 4.26 mmol) followed by methanesulfonyl chloride (256 μl, 3.41 mmol). After stirring for 1.5 hr., the mixture was diluted with dichloromethane, washed with aqueous saturated sodium bicarbonate solution, dried with anhydrous magnesium sulfate, filtered, and evaporated in vacuo. The residue was further dried in high vacuo and mixed with compound 8 (945 mg, 2.84 mmol), anhydrous powdered potassium carbonate (392 mg, 2.84 mmol), and lithium iodide (381 mg, 2.84 mmol). Anhydrous DMF (15 ml) was then added into the mixture and stirred for overnight at room temperature. The mixture was evaporated in vacuo. The residue was dissolved in methanol-dichloromethane (1:9), filtered through a celite pad, and the pad was washed with dichloromethane. The combined filtrate was evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, EA:hexanes (1:2)) to afford 963 mg (57%) of a white foam. 1H NMR (200 MHz, CDCl3) δ 1.11 (6H, d, J=7.0 Hz), 2.30 (3H, s), 2.72 (1H, m), 3.79 (3H, s), 3.93-4.06 (4H, m), 4.30 (2H, d, J=5.4 Hz), 4.67 (2H, s), 5.04 (1H, t, J=5.4 Hz), 5.67 (1H, s), 5.96 (1H, s), 6.36 (1H, s), 6.57 (1H, s), 6.79 (1H, s), 6.85 (2H, d, J=8.4 Hz), 7.01 (1H, s), 7.22 (2H, d, J=8.4 Hz), 9.01 (1H, s).

後処理

  1. washwashed with aqueous saturated sodium bicarbonate solution
  2. dry with materialdried with anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customThe residue was further dried in high vacuo
  6. stirringstirred for overnight at room temperature
  7. customThe mixture was evaporated in vacuo
  8. dissolutionThe residue was dissolved in methanol-dichloromethane (1:9)
  9. filtrationfiltered through a celite pad
  10. washthe pad was washed with dichloromethane
  11. customThe combined filtrate was evaporated in vacuo
  12. customthe residue was purified by silica gel column chromatography (eluent, EA:hexanes (1:2))

出典と根拠

ORDレコード
ord-16c7f40ddeb2407181158171f79cfa16
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08106064B2

反応ノート

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