Potassium Carbonate → 2-(p-benzoylphenoxy)ethylthiocarbamic acid S-ethyl ester

HRID 2058270노트

반응식

HRID 2058270 반응식
[C:1]([C:9]1[CH:18]=[CH:17][C:12]([O:13][CH2:14][CH2:15][NH2:16])=[CH:11][CH:10]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:19]([S:21][C:22](Cl)=[O:23])[CH3:20].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:19]([S:21][C:22](=[O:23])[NH:16][CH2:15][CH2:14][O:13][C:12]1[CH:11]=[CH:10][C:9]([C:1](=[O:8])[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[CH:18][CH:17]=1)[CH3:20]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 18056Ethyl chlorothioformateHCID 3393464[4-(2-Aminoethoxy)phenyl]-phenylmethanone

생성물 1

HCID 544080062-(p-benzoylphenoxy)ethylthiocarbamic acid S-ethyl ester

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

6.4 g of 2-(p-benzoylphenoxy)ethylamine and 17.2 g of chlorothioformic acid S-ethyl ester are dissolved in 230 ml of acetone, 22.2 g of potassium carbonate are added to the solution. The mixture is heated under reflux for 6 hours. After cooling to room temperature, the mixture is filtered, the residue is washed with acetone and the filtrate is evaporated in vacuo. The residue is suspended in hot ether and filtered. The residue is then washed with ether and the filtrate is evaporated in vacuo. Recrystallization of the residue from ether yields 2-(p-benzoylphenoxy)ethylthiocarbamic acid S-ethyl ester, m.p.--90°-92° C. Recrystallization of the mother liquor yields a further 1 g of product.

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 6 hours
  3. filtrationthe mixture is filtered
  4. washthe residue is washed with acetone
  5. customthe filtrate is evaporated in vacuo
  6. filtrationfiltered
  7. washThe residue is then washed with ether
  8. customthe filtrate is evaporated in vacuo
  9. customRecrystallization of the residue from ether

출처 및 근거

ORD 기록
ord-6556363d727545f7aa14116f3f4029a6
출처 데이터셋
uspto-grants-1980_07
특허 번호
US04215139

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