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Hydrochloric Acid → HCID 178478870、化合物

HRID 1285335
ノート
印刷プレビュー

反応式

HRID 1285335 の反応式
I.[CH2:2]([N:9]1[CH2:13][C:12](=[O:14])[N:11]=[C:10]1SC)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[N:17]1([CH2:23][C:24]2[CH:25]=[C:26]([CH:32]=[CH:33][CH:34]=2)[O:27][CH2:28][CH2:29][CH2:30][NH2:31])[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1.C(N(CC)CC)C.[ClH:42]>C(O)C>[ClH:42].[ClH:42].[N:17]1([CH2:23][C:24]2[CH:25]=[C:26]([CH:32]=[CH:33][CH:34]=2)[O:27][CH2:28][CH2:29][CH2:30][NH:31][C:10]2[N:9]([CH2:2][C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=3)[CH2:13][C:12](=[O:14])[N:11]=2)[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 102205613-(3-(Piperidin-1-ylmethyl)phenoxy)propan-1-amineHCID 20248961HCID 20248961、化合物

生成物 1

HCID 178478870HCID 178478870、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-Benzyl-2-methylthio-2-imidazolin-4-one hydroiodide (2.09 g) from the previous stage, 3-(3-piperidinomethylphenoxy)propylamine (1.49 g) and triethylamine (1.27 g) were refluxed in ethanol (35 ml) for 7 hours with stirring. The solution was allowed to cool overnight and evaporated under reduced pressure to give a residue. This residue was dissolved in 2N hydrochloric acid (30 ml), and extracted with chloroform (3×20 ml). The aqueous layer was taken to pH 10 with 2N sodium hydroxide and extracted with chloroform (3×30 ml). The latter chloroform extracts were dried (MgSO4) and evaporated under reduced pressure. The residue was washed thoroughly with cold diethyl ether and treated with dilute ethanolic HCL. Excess solvent was evaporated and the residue recrystallised from isopropanolacetone to afford 2-[3-(3-piperidinomethylphenoxy)propylamino]-1-benzylimidazolin-4-one dihydrochloride, m.p. 95°-98° C.

後処理

  1. temperatureto cool overnight
  2. customevaporated under reduced pressure
  3. customto give a residue
  4. extractionextracted with chloroform (3×20 ml)
  5. extractionextracted with chloroform (3×30 ml)
  6. dry with materialThe latter chloroform extracts were dried (MgSO4)
  7. customevaporated under reduced pressure
  8. washThe residue was washed thoroughly with cold diethyl ether
  9. additiontreated with dilute ethanolic HCL
  10. customExcess solvent was evaporated
  11. customthe residue recrystallised from isopropanolacetone

出典と根拠

ORDレコード
ord-12fe3a3c0fc741e0a2435b6dacfae28f
出典データセット
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04567176

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート