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

HRID 461111ノート

反応式

HRID 461111 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4fbf59d8134e4cd6a7123834d08ab33b
出典データセット
uspto-grants-1977_12
特許番号
US04061761

反応ノート

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