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Hydrochloric Acid → HCID 21183852、化合物

HRID 1384840
ノート
印刷プレビュー

反応式

HRID 1384840 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 600381HCID 600381、化合物HCID 9899402N-(2-Methoxyphenyl)piperazine hydrochloride

生成物 1

HCID 21183852HCID 21183852、化合物収率 10%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 3283
Diethyl Ether
溶媒

実験手順

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%.

後処理

  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)

出典と根拠

ORDレコード
ord-5c5578cbc90543d1acf45c751de06abd
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06262056B1

反応ノート

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