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Ethyl Thioglycolate → HCID 21241315, 화합물

HRID 1761428
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HRID 1761428 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

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

생성물 1

HCID 21241315HCID 21241315, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매
HCID 6344
Dichloromethane
용매
2회

실험 절차

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.

후처리

  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]

출처 및 근거

ORD 기록
ord-3715ae08be1442abba4548a5a4379b28
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04826834

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