Ammonia → N-[2-(4-Carboethoxymethoxyphenyl)-1-methylethyl]-2-(2-trifluoromethyl-thiazol-4yl)morpholine hydrochloride

HRID 1451441노트

반응식

HRID 1451441 반응식
[C:1]([CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH:13]([N:15]2[CH2:20][CH2:19][O:18][CH:17]([C:21]3[N:22]=[C:23]([C:26]([F:29])([F:28])[F:27])[S:24][CH:25]=3)[CH2:16]2)[CH3:14])=[CH:8][CH:7]=1)([OH:3])=[O:2].[CH2:30](O)[CH3:31].S(=O)(=O)(O)O.N.C(Cl)(Cl)[Cl:40]>>[ClH:40].[C:1]([CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][CH:13]([N:15]2[CH2:20][CH2:19][O:18][CH:17]([C:21]3[N:22]=[C:23]([C:26]([F:27])([F:28])[F:29])[S:24][CH:25]=3)[CH2:16]2)[CH3:14])=[CH:8][CH:7]=1)([O:3][CH2:30][CH3:31])=[O:2]

참가 물질

6

반응물 5

HCID 222AmmoniaHCID 702EthanolHCID 1118Sulfuric AcidHCID 6212ChloroformHCID 19974278N-[2-(4-Carboxymethoxyphenyl)-1-methylethyl]-2-(2-trifluoromethyl-thiazol-4-yl)morpholine

생성물 1

HCID 19974260N-[2-(4-Carboethoxymethoxyphenyl)-1-methylethyl]-2-(2-trifluoromethyl-thiazol-4yl)morpholine hydrochloride

실험 절차

0.5 g (0.0012 mol) of N-[2-(4-carboxymethoxyphenyl)-1-methylethyl]-2-(2-trifluoromethyl-thiazol-4-yl)morpholine is dissolved in 150 ml of chloroform and, while stirring, 2 ml ethanol and 0.25 g of concentrated sulphuric acid are added, and the mixture is heated to reflux with a water trap for one hour. The mixture is then cooled, ice-water is added, the mixture is made alkaline with ammonia and the phases are separated. The aqueous phase is then extracted again by shaking with chloroform, and the organic phase is dried over sodium sulphate, filtered and evaporated to dryness. The resulting residue is dissolved in ether, ethereal hydrochloric acid is added, the mixture is evaporated to dryness, and the residue is triturated with acetone and filtered off with suction.

후처리

  1. temperaturethe mixture is heated
  2. temperatureto reflux with a water trap for one hour
  3. temperatureThe mixture is then cooled
  4. customthe phases are separated
  5. extractionThe aqueous phase is then extracted again
  6. stirringby shaking with chloroform
  7. dry with materialthe organic phase is dried over sodium sulphate
  8. filtrationfiltered
  9. customevaporated to dryness
  10. dissolutionThe resulting residue is dissolved in ether
  11. additionethereal hydrochloric acid is added
  12. customthe mixture is evaporated to dryness
  13. customthe residue is triturated with acetone
  14. filtrationfiltered off with suction

출처 및 근거

ORD 기록
ord-f38e57dcd18441adb2334862f8d3b5dc
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05604225

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