Hydrochloric Acid → 1-Benzyl-3-(1,3-dithiol-2-ylidene)-2,4-dioxopiperidine

HRID 977955ノート

反応式

HRID 977955 の反応式
[CH2:1]([N:8]1[C:13](=[O:14])[C:12](=[C:15]2[S:19][CH:18]=[CH:17][S:16]2)[C:11](=[O:20])[CH:10](C(OCC)=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].Cl>C(O)C>[CH2:1]([N:8]1[CH2:9][CH2:10][C:11](=[O:20])[C:12](=[C:15]2[S:16][CH:17]=[CH:18][S:19]2)[C:13]1=[O:14])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 13934862Ethyl 1-benzyl-5-(1,3-dithiol-2-ylidene)-4,6-dioxopiperidine-3-carboxylate

生成物 1

HCID 136065591-Benzyl-3-(1,3-dithiol-2-ylidene)-2,4-dioxopiperidine収率 78%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl 1-benzyl-5-(1,3-dithiol-2-ylidene)-4,6-dioxopiperidine-3-carboxylate (2.0 g) is dissolved in ethanol (160 ml), and a 10% aqueous sodium hydroxide solution (8.0 ml) is added thereto. The mixture is refluxed for 2 hours. The mixture is cooled, neutralized with 10% hydrochloric acid, and then evaporated under reduced pressure to remove the solvent. The residue is dissolved in ethyl acetate, and the solution is washed with water, dried and then evaporated to remove the solvent. The residue thus obtained is recrystallized from isopropanol, whereby 1-benzyl-3-(1,3-dithiol-2-ylidene)-2,4-dioxopiperidine (1.26 g) is obtained as pale yellow needles. Yield: 78%.

後処理

  1. temperatureThe mixture is refluxed for 2 hours
  2. temperatureThe mixture is cooled
  3. customevaporated under reduced pressure
  4. customto remove the solvent
  5. dissolutionThe residue is dissolved in ethyl acetate
  6. washthe solution is washed with water
  7. customdried
  8. customevaporated
  9. customto remove the solvent
  10. customThe residue thus obtained
  11. customis recrystallized from isopropanol

出典と根拠

ORDレコード
ord-37a9a66402b8473f8bd98f6f8567048c
出典データセット
uspto-grants-1987_05
特許番号
US04663319

反応ノート

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