Formaldehyde → Methyl 4-(6-propyloxycarbonyl-2,3,4-trihydroxybenzyl)-1-piperazinecarbodithioate

HRID 1460169

반응식

HRID 1460169 반응식
[CH2:1]=O.[N:3]1([C:9]([S:11][CH3:12])=[S:10])[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.[C:13]([O:24][CH2:25][CH2:26][CH3:27])(=[O:23])[C:14]1[CH:22]=[C:20]([OH:21])[C:18]([OH:19])=[C:16]([OH:17])[CH:15]=1>C(O)C>[CH2:25]([O:24][C:13]([C:14]1[C:15]([CH2:1][N:6]2[CH2:7][CH2:8][N:3]([C:9]([S:11][CH3:12])=[S:10])[CH2:4][CH2:5]2)=[C:16]([OH:17])[C:18]([OH:19])=[C:20]([OH:21])[CH:22]=1)=[O:23])[CH2:26][CH3:27]

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 4947Propyl GallateHCID 21278808Methyl piperazine-1-carbodithioate

생성물 1

HCID 53992097Methyl 4-(6-propyloxycarbonyl-2,3,4-trihydroxybenzyl)-1-piperazinecarbodithioate수율 46%

시약·촉매·용매 1

HCID 702Ethanol용매3회

실험 절차

In 10 ml of ethanol was dissolved 0.86 g (10 mmol.) of 35% formalin. To the solution placed in an ice bath was further added a solution of 1.94 g (10 mmol., purity 90.7%) of methyl 1-piperazinecarbodithioate in 4 ml of ethanol. The resulting mixture was then stirred for 30 min. at room temperature. To the mixture placed in an ice bath was dropwise added a solution of 2.12 g (10 mmol.) of propyl gallate in 4 ml of ethanol. The mixture was stirred overnight at room temperature and subsequently refluxed under heating for 4 hours. The mixture was cooled to room temperature. Precipitated crystals were collected by filtration and washed with ethanol to give 1.843 g of the desired compound as a grayish powder, m.p. 142°-144° C. (decomp.), yield 31.3%.

후처리

  1. customTo the solution placed in an ice bath
  2. customTo the mixture placed in an ice bath
  3. stirringThe mixture was stirred overnight at room temperature
  4. temperaturesubsequently refluxed
  5. temperatureunder heating for 4 hours
  6. temperatureThe mixture was cooled to room temperature
  7. customPrecipitated crystals
  8. filtrationwere collected by filtration
  9. washwashed with ethanol

출처 및 근거

ORD 기록
ord-38f3fecb76b842b19ae3a308b99b1144
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05070089

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