2,3-Dichlorobenzaldehyde → 5-[(2,3-Dichlorophenyl)methylene]-2-thioxo-4-thiazolidinone

HRID 128727

反応式

HRID 128727 の反応式
[Cl:1][C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.[S:11]1[CH2:17][C:15](=[O:16])[NH:14][C:12]1=[S:13].C([O-])(=O)C.[Na+]>C(O)(=O)C>[Cl:1][C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[C:17]1[S:11][C:12](=[S:13])[NH:14][C:15]1=[O:16]

参加物

5

反応物 3

HCID 357452,3-DichlorobenzaldehydeHCID 517045Sodium AcetateHCID 1201546Rhodanine

生成物 1

HCID 28543725-[(2,3-Dichlorophenyl)methylene]-2-thioxo-4-thiazolidinone収率 40%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 2,3-dichlorobenzaldehyde (4.6 g, mmoles), rhodanine (3.5 g, 25 mmoles), sodium acetate (7.5 g, 91 mmoles), and acetic acid (40 ml) is stirred under an inert atmosphere and heated to reflux. After 2.5 hours the mixture is stirred into ice-water (250 ml) and the precipitate is filtered off, rinsed three times with water and dried. Recrystallization from methanol gave the pure product (2.9 g), mp 203°-204° C.

後処理

  1. temperatureheated to reflux
  2. filtrationthe precipitate is filtered off
  3. washrinsed three times with water
  4. customdried
  5. customRecrystallization from methanol

出典と根拠

ORDレコード
ord-029bb7e8f5a3430fb8eff75b0d44cb04
出典データセット
uspto-grants-1995_11
特許番号
US05464856

関連ノート

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