Sodium hydride → HCID 57779569、化合物

HRID 509202

反応式

HRID 509202 の反応式
[I-].[CH3:2][S+](C)(C)=O.[H-].[Na+].[C:9]([CH:17]1[CH2:22][CH2:21][N:20]([C:23]([O:25][CH2:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[O:24])[CH2:19][CH2:18]1)(=[O:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C1COCC1>[C:10]1([C:9]2([CH:17]3[CH2:18][CH2:19][N:20]([C:23]([O:25][CH2:26][C:27]4[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=4)=[O:24])[CH2:21][CH2:22]3)[CH2:2][O:16]2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 74498Sulfoxonium, trimethyl-, iodide (1:1)HCID 57779495Benzyl 4-benzoylpiperidine-1-carboxylate

生成物 1

HCID 57779569HCID 57779569、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
55 °C

実験手順

A mixture of trimethylsulfoxonium iodide (2.402 g, 10.91 mmol) and sodium hydride (0.436 g, 10.91 mmol) in THF (20 mL) was heated at 55° C. for 3 h then a solution of compound 87 (2.82 g, 8.73 mmol) in THF (10 mL) was added. The reaction mixture was stirred for 36 h, quenched with water, extracted with ether and the combined organics were washed with water, brine, dried over Na2SO4, filtered and concentrated to afford compound 88 used as a crude in the next step.

後処理

  1. customquenched with water
  2. extractionextracted with ether
  3. washthe combined organics were washed with water, brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-47a0692d80a84ad6abc82a1fbdd45245
出典データセット
uspto-grants-2015_08
特許番号
US09096565B2

関連ノート

読み込み中…