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Lithium Hexamethyldisilazide → 2-Propen-1-yl {3-[(2-chloro-4-pyrimidinyl)acetyl]-2-fluorophenyl}carbamate

HRID 1670926
ノート
印刷プレビュー

反応式

HRID 1670926 の反応式
[CH2:1]([O:4][C:5]([NH:7][C:8]1[C:9]([F:18])=[C:10]([CH:15]=[CH:16][CH:17]=1)[C:11]([O:13]C)=O)=[O:6])[CH:2]=[CH2:3].[Li+].[CH3:20][Si]([N-][Si](C)(C)C)(C)C.[Cl-:29].[N:30]1[CH:35]=[CH:34][CH:33]=[N:32][CH:31]=1>C1COCC1>[Cl:29][C:31]1[N:32]=[C:33]([CH2:20][C:11]([C:10]2[C:9]([F:18])=[C:8]([NH:7][C:5](=[O:6])[O:4][CH2:1][CH:2]=[CH2:3])[CH:17]=[CH:16][CH:15]=2)=[O:13])[CH:34]=[CH:35][N:30]=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

5

反応物 3

HCID 2733832Lithium HexamethyldisilazideHCID 22046915Pyrimidine chlorideHCID 57989974Methyl 3-(allyloxycarbonylamino)-2-fluorobenzoate

生成物 1

HCID 579899922-Propen-1-yl {3-[(2-chloro-4-pyrimidinyl)acetyl]-2-fluorophenyl}carbamate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of methyl 3-(allyloxycarbonylamino)-2-fluorobenzoate (86.7 g, 342 mmol, 1 eq) in dry THF (500 mL) at −10° C., LiHMDS (1M in THF, 1198 mmol, 1198 mL, 3.5 eq) was added dropwise and the solution was allowed to stir for 1 h at 0° C. A solution of pyrimidine chloride (48.0 g, 376 mmol, 1.2 eq) in THF (200 mL) was then added dropwise to the solution of ester and base at 0° C. over 20 min. The solution was allowed to stir 1 h at rt. TLC showed the reaction was complete. The reaction was quenched by addition of the saturated aqueous NH4Cl (800 mL) at 0° C. The reaction mixture was extracted with EtOAc (1 L×3). The combined organic layers were washed with water and brine successively, dried over Na2SO4, filtered and concentrated under reduced pressure to give the crude product, which was purified by flash column on silica gel, rinsing with DCM. This solution was concentrated to obtain a solid. The orange solid was triturated with a small amount of EtOAc and filtered, rinsing with diethyl ether to give the product (240.1 g, 67.0%, three batches combined). 1H NMR (400 MHz, DMSO-d6) δ ppm 13.70 (s, 1H), 8.52 (dd, J=0.8, 4.8 Hz, 0.3H), 8.34 (dd, J=0.8, 5.2 Hz, 1H), 8.27 (s, 0.4H), 8.10 (s, 1H), 7.47 (t, J=8.0 Hz, 1.4H), 7.22-7.12 (m, 1.8H), 6.96 (s, 1.4H), 6.85 (d, J=4.2 Hz, 1H), 6.07 (s, 1H), 5.97-5.86 (m, 1.4H), 5.32 (d, J=15.6 Hz, 1.4H), 5.24 (d, J=6.4 Hz, 1.4H), 4.64 (d, J=6.0 Hz, 2.8H), 4.38 (d, J=2.8 Hz, 0.8H).

後処理

  1. stirringto stir 1 h at rt
  2. customThe reaction was quenched by addition of the saturated aqueous NH4Cl (800 mL) at 0° C
  3. extractionThe reaction mixture was extracted with EtOAc (1 L×3)
  4. washThe combined organic layers were washed with water and brine successively
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-ad1247e6ba40434eb5f43ef67a64dca6
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07994185B2

反応ノート

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