Piperidine → 5-[2-(3-Phenylureido)thiazol-4-ylmethylene]rhodanine-3-acetic acid

HRID 2107171ノート

反応式

HRID 2107171 の反応式
[C:1]1([NH:7][C:8](=[O:17])[NH:9][C:10]2[S:11][CH:12]=[C:13]([CH:15]=O)[N:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[S:18]1[CH2:24][C:22](=[O:23])[N:21]([CH2:25][C:26]([OH:28])=[O:27])[C:19]1=[S:20].N1CCCCC1>C(O)C>[C:1]1([NH:7][C:8](=[O:17])[NH:9][C:10]2[S:11][CH:12]=[C:13]([CH:15]=[C:24]3[S:18][C:19](=[S:20])[N:21]([CH2:25][C:26]([OH:28])=[O:27])[C:22]3=[O:23])[N:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 8082PiperidineHCID 797933-Thiazolidineacetic acid, 4-oxo-2-thioxo-HCID 150535142-(3-Phenylureido)thiazole-4-carbaldehyde

生成物 1

HCID 544121855-[2-(3-Phenylureido)thiazol-4-ylmethylene]rhodanine-3-acetic acid収率 45.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture comprising 1 g of 2-(3-phenylureido)thiazole-4-carbaldehyde, 0.85 g of rhodanine-3-acetic acid, 0.76 g of piperidine and 15 ml of ethanol was stirred at room temperature for 2 hours, and the resulting mixture was left to stand overnight. The crystals which precipitated out were collected by filtration dispersed in dilute aqueous hydrochloric acid, and washed with stirring for 30 minutes. The resulting crystalline product was recrystallized from a mixture of acetic acid and ethyl acetate, giving 0.78 g of the desired compound as an orange powder.

後処理

  1. waitthe resulting mixture was left
  2. waitto stand overnight
  3. customThe crystals which precipitated out
  4. filtrationwere collected by filtration
  5. additiondispersed in dilute aqueous hydrochloric acid
  6. washwashed
  7. stirringwith stirring for 30 minutes
  8. customThe resulting crystalline product was recrystallized from a mixture of acetic acid and ethyl acetate

出典と根拠

ORDレコード
ord-7b4ddc6af69b4c5999e9c08d89975569
出典データセット
uspto-grants-1990_06
特許番号
US04933355

反応ノート

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