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

HRID 2107171노트

반응식

HRID 2107171 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7b4ddc6af69b4c5999e9c08d89975569
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04933355

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