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Ethyl Thioglycolate → HCID 21241315、化合物

HRID 1761428
ノート
印刷プレビュー

反応式

HRID 1761428 の反応式
[CH3:1][CH2:2][O:3][C:4]([CH2:6][SH:7])=[O:5].[H-].[Na+].Cl[C:11]1[N:16]2[N:17]=[CH:18][N:19]=[C:15]2[N:14]=[C:13]([CH3:20])[CH:12]=1>C(O)C.ClCCl.O>[CH2:2]([O:3][C:4]([CH2:6][S:7][C:11]1[N:16]2[N:17]=[CH:18][N:19]=[C:15]2[N:14]=[C:13]([CH3:20])[CH:12]=1)=[O:5])[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 12185Ethyl ThioglycolateHCID 24758Sodium hydrideHCID 5201277-Chloro-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidine

生成物 1

HCID 21241315HCID 21241315、化合物

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

Ethyl thioglycollate, 1.2 g, is dissolved in 30 ml of dry ethanol, to which 400 mg of sodium hydride (60% in an oil) is added under cooling with ice water and stirred for 10 minutes. Then 1.7 g of 7-chloro-5-methyl-[1,2,4]triazolo[1,5-a]pyrimidine and 10 ml of dry dichloromethane are added and stirred for 16 hours. To the reaction mixture, water and dichloromethane are added and the organic layer is separated. The separated organic layer is washed with saline and dried over anhydrous potassium carbonate. The solvent is evaporated under reduced pressure and the residue is purified by column chromatography [on 40 g of silica gel, developed and eluted with ethyl acetate] to give 2.2 g of the desired compound as a colorless powder.

後処理

  1. additionis added
  2. stirringstirred for 16 hours
  3. customthe organic layer is separated
  4. washThe separated organic layer is washed with saline
  5. dry with materialdried over anhydrous potassium carbonate
  6. customThe solvent is evaporated under reduced pressure
  7. customthe residue is purified by column chromatography [on 40 g of silica gel, developed and eluted with ethyl acetate]

出典と根拠

ORDレコード
ord-3715ae08be1442abba4548a5a4379b28
出典データセット
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04826834

反応ノート

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