Triethylamine → 3-Ethyl-2-ethylimino-4-(4-chloro-3-sulfamoylphenyl)-1,3-thiazolidine-4-ol-hydrochloride

HRID 461111노트

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HRID 461111 반응식
Br.[CH2:2]([N:4]1[C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:11]=2)([OH:9])[CH2:7][S:6][C:5]1=[N:21][CH2:22][CH3:23])[CH3:3].C(N(CC)CC)C>CO>[ClH:16].[CH2:2]([N:4]1[C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:11]=2)([OH:9])[CH2:7][S:6][C:5]1=[N:21][CH2:22][CH3:23])[CH3:3]

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 227605773-Ethyl-2-ethylimino-4-(4-chloro-3-sulfamoylphenyl)-1,3-thiazolidine-4-ol-hydrobromide

생성물 1

HCID 227605293-Ethyl-2-ethylimino-4-(4-chloro-3-sulfamoylphenyl)-1,3-thiazolidine-4-ol-hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

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온도
40 °C

실험 절차

17 g of 3-ethyl-2-ethylimino-4-(4-chloro-3-sulfamoylphenyl)-1,3-thiazolidine-4-ol-hydrobromide were suspended in 100 ml of methanol and shortly heated to boiling after the addition of 10 ml of triethyl amine. The solvent was distilled off under reduced pressure, 150 ml of water were added to the residue and the mixture was extracted with 200 ml of ethyl acetate. After drying the organic phase over sodium sulfate the solvent was distilled off under reduced pressure. The residue was dissolved in 100 ml of acetone, the solution was acidified with 15% ethanolic HCl and the oily precipitate of the end product was crystallized with acetone heated to 40° C.

후처리

  1. temperatureshortly heated
  2. distillationThe solvent was distilled off under reduced pressure, 150 ml of water
  3. additionwere added to the residue
  4. extractionthe mixture was extracted with 200 ml of ethyl acetate
  5. dry with materialAfter drying the organic phase over sodium sulfate the solvent
  6. distillationwas distilled off under reduced pressure
  7. dissolutionThe residue was dissolved in 100 ml of acetone
  8. customthe oily precipitate of the end product was crystallized with acetone

출처 및 근거

ORD 기록
ord-4fbf59d8134e4cd6a7123834d08ab33b
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061761

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