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Hydrochloric Acid → HCID 21183852, 화합물

HRID 1384840
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HRID 1384840 반응식
[C:1]([C:4]1[C:5]2[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:6]=2[S:7][CH:8]=1)(=[O:3])[CH3:2].[ClH:14].[CH3:15][O:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.Cl.[CH2:30]=O>CCO.C(OCC)C>[ClH:14].[ClH:14].[CH3:13][C:11]1[CH:10]=[CH:9][C:6]2[S:7][CH:8]=[C:4]([C:1](=[O:3])[CH2:2][CH2:30][N:26]3[CH2:27][CH2:28][N:23]([C:18]4[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=4[O:16][CH3:15])[CH2:24][CH2:25]3)[C:5]=2[CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 600381HCID 600381, 화합물HCID 9899402N-(2-Methoxyphenyl)piperazine hydrochloride

생성물 1

HCID 21183852HCID 21183852, 화합물수율 10%

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 3283
Diethyl Ether
용매

실험 절차

650 mg of 3-acetyl-5-methylbenzo[b]thiophene (3.42×10−3 moles) and 860 mg of 2-methoxyphenylpiperazine hydrochloride (3.76×10−3 moles) were dissolved in 15 ml of EtOH and HCl to pH=2-3. When the mixture was under reflux, 310 mg of paraformaldehyde (10×10−3 moles) were added. After 24 hours stirring under reflux the reaction mixture was poured over ice and was extracted with AcOEt. It was washed with H2O and dried with Na2SO4, the solvent being removed to dryness. It was purified in silica column using AcOEt/hexane (1:1) as mobile phase. The oil obtained was dissolved in ethyl ether (20 ml) and EtOH (4 ml) and precipitates as hydrochloride on adding HCl(c). Yield: 10%.

후처리

  1. temperatureunder reflux
  2. temperatureunder reflux the reaction mixture
  3. additionwas poured over ice
  4. extractionwas extracted with AcOEt
  5. washIt was washed with H2O
  6. dry with materialdried with Na2SO4
  7. customthe solvent being removed to dryness
  8. customIt was purified in silica column
  9. customThe oil obtained
  10. customEtOH (4 ml) and precipitates as hydrochloride
  11. additionon adding HCl(c)

출처 및 근거

ORD 기록
ord-5c5578cbc90543d1acf45c751de06abd
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06262056B1

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