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Formaldehyde → Methyl 4-(2-hydroxy-5-methoxybenzyl)-1-piperazinecarbodithioate

HRID 1757532
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HRID 1757532 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.[CH3:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([OH:21])=[CH:17][CH:16]=1>C(O)C>[OH:21][C:18]1[CH:19]=[CH:20][C:15]([O:14][CH3:13])=[CH:16][C:17]=1[CH2:1][N:6]1[CH2:7][CH2:8][N:3]([C:9]([S:11][CH3:12])=[S:10])[CH2:4][CH2:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 90154-MethoxyphenolHCID 21278808Methyl piperazine-1-carbodithioate

생성물 1

HCID 19388436Methyl 4-(2-hydroxy-5-methoxybenzyl)-1-piperazinecarbodithioate수율 34%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 20 ml of ethanol was 1.05 g of 37% formalin, and to the mixture was added under chilling with ice 2.29 g of methyl 1-piperazinecarbodithioate.The mixture was then stirred for 30 min. at room temperature, and, after addition of 1.24 g of 4-methoxyphenol, refluxed overnight under heating. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography. The obtained oil was crystallized from 10 ml of ethanol. The crystals were collected by filtration and subsequently washed with ethanol to give 1.06 g of the desired compound as white crystals, m.p. 112° C., yield 34%.

후처리

  1. additionto the mixture was added
  2. temperaturerefluxed overnight
  3. temperatureunder heating
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe residue was purified by silica gel column chromatography
  6. customThe obtained oil was crystallized from 10 ml of ethanol
  7. filtrationThe crystals were collected by filtration
  8. washsubsequently washed with ethanol

출처 및 근거

ORD 기록
ord-ff4d30981a7a4a5692f88990382ebfac
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05446146

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