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Sodium hydride → HCID 53830736、化合物

HRID 1432933
ノート
印刷プレビュー

反応式

HRID 1432933 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][NH:14][C:13](=[O:17])[C@@H:12]1[CH3:18])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I-].[H-].[Na+].Br[CH2:23][C:24]1[CH:33]=[C:32]2[C:27]([C:28]([Cl:34])=[CH:29][CH:30]=[N:31]2)=[CH:26][CH:25]=1>C1COCC1>[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][N:14]([CH2:23][C:24]2[CH:33]=[C:32]3[C:27]([C:28]([Cl:34])=[CH:29][CH:30]=[N:31]3)=[CH:26][CH:25]=2)[C:13](=[O:17])[C@@H:12]1[CH3:18])=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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

6

反応物 4

HCID 24758Sodium hydrideHCID 30165Iodide IonHCID 217084447-Bromomethyl-4-chloroquinolineHCID 542270461-Piperazinecarboxylic acid, 2-methyl-3-oxo-, phenylmethyl ester, (2S)-

生成物 1

HCID 53830736HCID 53830736、化合物収率 77.5%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

反応条件

温度
0 °C

実験手順

4-(Benzyloxycarbonyl)-3-(S)-methylpiperazin-2-one (1.0 g, 4.0 mmol), EXAMPLE 46, is dissolved in THF (60 mL), cooled in an ice bath and treated with tretrabutylammonium iodide (0.10 g, 0.27 mmol) and 60% sodium hydride (0.18 g, 4.4 mmol). The reaction mixture is stirred at 0° C. for 30 minutes then treated dropwise with a solution of 7-bromomethyl-4-chloroquinoline (1.12 g, 4.4 mmol), EXAMPLE 14, in THF (5 mL). The resulting solution warmed to room temperature over approximately 1 h then quenched with sodium bicarbonate solution and concentrated. The residue is partitioned between ethyl acetate and water; the organic layer is dried (sodium sulfate) and concentrated. The residue is chromatographed (5% methanol/methylene chloride) to yield solid 4-(Benzyloxycarbonyl)-1-(4-chloroquinolin-7-ylmethyl)-3-(S)-methyl-piperazin-2-one (1.32 g, 3.1 mmol). A portion of this material (0.10 g, 0.23 mmol) is dissolved in acetonitrile (6 mL) and treated with iodotrimethyl-silane (0.1 mL, 0.75 mmol) at room temperature for 2 hours. The reaction is quenched with methanol and concentrated to dryness. Methanol addition and concentration is repeated six times. The final residue is taken up is 2M aqueous HCl; the solution is washed with ether and concentrated to yield the title compound. MS m/z: M+=289; 1H NMR (CD3OD, 300 MHz) δ9.2 (d, 1H), 8.6 (d, 1H), 8.2-8.3 (m, 2H), 8.0 (d, 1H), 5.1 (q, 1H), 4.3-4.4 (m, 1H), 3.8-4.0 (m, 2H), 3.6-3.8 (m, 3H), 1.75 (d, 3H).

後処理

  1. temperaturecooled in an ice bath
  2. temperatureThe resulting solution warmed to room temperature over approximately 1 h
  3. customthen quenched with sodium bicarbonate solution
  4. concentrationconcentrated
  5. customThe residue is partitioned between ethyl acetate and water
  6. dry with materialthe organic layer is dried (sodium sulfate)
  7. concentrationconcentrated
  8. customThe residue is chromatographed (5% methanol/methylene chloride)

出典と根拠

ORDレコード
ord-fdb07ba2bcdd47d89688c2cdbc9d31d7
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07612075B2

反応ノート

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