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2,4,6-Trimethylbenzyl chloride → HCID 178492802、化合物

HRID 2216307
ノート
印刷プレビュー

反応式

HRID 2216307 の反応式
[Mg].[CH3:2][C:3]1[CH:10]=[C:9]([CH3:11])[CH:8]=[C:7]([CH3:12])[C:4]=1[CH2:5]Cl.CC1C=C(C)C=C(C)C=1C[Mg]Cl.[CH3:25][O:26][C:27]1[CH:32]=[CH:31][C:30]([S:33]([C:36]2[CH:37]=[N:38][C:39]([CH3:42])=[N:40][CH:41]=2)(=[O:35])=[O:34])=[CH:29][CH:28]=1>CCOCC.C1COCC1>[CH3:25][O:26][C:27]1[CH:28]=[CH:29][C:30]([S:33]([C:36]2[CH:41]([CH2:5][C:4]3[C:3]([CH3:2])=[CH:10][C:9]([CH3:11])=[CH:8][C:7]=3[CH3:12])[NH:40][C:39]([CH3:42])=[N:38][CH:37]=2)(=[O:35])=[O:34])=[CH:31][CH:32]=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

7

反応物 4

HCID 741082,4,6-Trimethylbenzyl chlorideHCID 5462224MagnesiumHCID 21941673HCID 21941673、化合物HCID 178425038HCID 178425038、化合物

生成物 1

HCID 178492802HCID 178492802、化合物収率 51%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒3 回
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

To a mixture of magnesium (240 mg, 10 mmol) and ether (20 mL) was added 2,4,6-trimethylbenzyl chloride (1.69 g, 10 mmol) in ether (20 mL) dropwise at reflux under N2. The freshly prepared solution of 2,4,6-trimethylbenzylmagnesium chloride in ether was added to a solution of 5-(4-methoxy-benzenesulfonyl)-2-methylpyrimidine (264 mg, 1.0 mmol) in THF (10 mL) dropwise at 0° C. The mixture was stirred under N2 at 0° C. for 1 h and then quenched by addition of saturated aqueous NH4Cl. The organic layer was separated and the aqueous layer was extracted three times with EtOAc. The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by chromatography on silica gel (EtOAc) to provide 5-(4-methoxy-benzenesulfonyl)-2-methyl-6-(2,4,6-trimethylbenzyl)-1,6-dihydro-pyrimidine (203 mg, 51%) as a light yellow solid: 1H NMR (500 MHz, CDCl3) δ 7.86 (d, J=9.0 Hz, 2H), 7.45 (s, 1H), 6.99 (d, J=9.0 Hz, 2H), 6.83 (s, 2H), 4.40 (dd, J=10.8, 3.2 Hz, 1H), 3.86 (s, 3H), 2.96 (dd, J=14.2, 10.8 Hz, 1H), 2.87 (dd, J=14.2, 3.2 Hz, 1H), 2.25 (s, 6H), 2.24 (s, 3H), 1.91 (s, 3H); ESI MS m/z 399 [(M+H)+, calcd for C22H27N2O3S, 399.2].

後処理

  1. temperatureat reflux under N2
  2. customquenched by addition of saturated aqueous NH4Cl
  3. customThe organic layer was separated
  4. extractionthe aqueous layer was extracted three times with EtOAc
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by chromatography on silica gel (EtOAc)

出典と根拠

ORDレコード
ord-2a0be911131241418fdbdf15da106603
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07112585B2

反応ノート

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