Hydrochloric Acid → 2-[{2-(1,3-Benzodioxol-5-yl)ethyl}dithio]ethyl nicotinate hydrochloride

HRID 2259768ノート

反応式

HRID 2259768 の反応式
[C:1]([O:9][CH2:10][CH2:11][S:12][S:13][CH2:14][CH2:15][C:16]1[CH:24]=[CH:23][C:19]2[O:20][CH2:21][O:22][C:18]=2[CH:17]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1.[ClH:25]>C(OCC)(=O)C>[ClH:25].[C:1]([O:9][CH2:10][CH2:11][S:12][S:13][CH2:14][CH2:15][C:16]1[CH:24]=[CH:23][C:19]2[O:20][CH2:21][O:22][C:18]=2[CH:17]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[N:4][CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 190016562-[{2-(1,3-Benzodioxol-5-yl)ethyl}dithio]ethyl nicotinate

生成物 1

HCID 190016842-[{2-(1,3-Benzodioxol-5-yl)ethyl}dithio]ethyl nicotinate hydrochloride

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

2.5 g of the 2-[{2-(1,3-benzodioxol-5-yl)ethyl}dithio]ethyl nicotinate prepared in Example 3 was dissolved in 20 ml of ethyl acetate, followed by the addition of a solution of hydrochloric acid in ethyl acetate. The mixture was distilled to remove the solvent. The residue was dissolved in a methanol/ethanol mixture, followed by the filtration. The filtrate was concentrated and recrystallized from an ethanol/isopropyl ether mixture to obtain 2.5 g of the title compound as a colorless crystal.

後処理

  1. distillationThe mixture was distilled
  2. customto remove the solvent
  3. dissolutionThe residue was dissolved in a methanol/ethanol mixture
  4. filtrationfollowed by the filtration
  5. concentrationThe filtrate was concentrated
  6. customrecrystallized from an ethanol/isopropyl ether mixture

出典と根拠

ORDレコード
ord-047da405f7584e79bdee316f33905407
出典データセット
uspto-grants-1995_12
特許番号
US05475024

反応ノート

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