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Ethyl Acetate → ME-3407

HRID 1089754
ノート
印刷プレビュー

反応式

HRID 1089754 の反応式
[CH2:1]([O:5][C:6]([CH2:8][S:9][C:10]1[S:11][C:12]2[C:17]([N:18]=1)=[CH:16][CH:15]=[CH:14][N:13]=2)=[O:7])[CH2:2][CH2:3][CH3:4].ClC1C=CC=C(C(OO)=[O:27])C=1.C(OCC)(=O)C>C(Cl)Cl>[CH2:1]([O:5][C:6]([CH2:8][S:9]([C:10]1[S:11][C:12]2[C:17]([N:18]=1)=[CH:16][CH:15]=[CH:14][N:13]=2)=[O:27])=[O:7])[CH2:2][CH2:3][CH3:4]
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 8857Ethyl AcetateHCID 70297m-Chloroperbenzoic acidHCID 150356882-[(n-Butoxycarbonylmethyl)thio]thiazolo[5,4-b]pyridine

生成物 1

HCID 6918179ME-3407収率 68.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-10 °C

実験手順

Dissolved in 50 ml of methylene chloride was 18.5 g of the compound obtained in Example 1, and the solution was cooled down to -10° C. 16.2 g of m-chloroperbenzoic acid (with a 70% purity) was added to the solution, which was in turn stirred at that temperature for 40 minutes. Ethyl acetate (600 ml) was added to the solution, which was then washed once with an aqueous solution of sodium thiosulfate, three times with sodium hydrogencarbonate and once with water, dried over magnesium sulfate, and distilled to remove the solvent. The residue was purified by silica gel column chromatography, and eluting with n-hexane-ethyl acetate (5:3 to 3:1) to obtain the title compound (13.4 g).

後処理

  1. washwas then washed once with an aqueous solution of sodium thiosulfate, three times with sodium hydrogencarbonate and once with water
  2. dry with materialdried over magnesium sulfate
  3. distillationdistilled
  4. customto remove the solvent
  5. customThe residue was purified by silica gel column chromatography
  6. washeluting with n-hexane-ethyl acetate (5:3 to 3:1)

出典と根拠

ORDレコード
ord-2aa131be26f949d2ba44165c7e74aa2a
出典データセット
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05079255

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート