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Hydrochloric Acid → HCID 12810954、化合物

HRID 2166539
ノート
印刷プレビュー

反応式

HRID 2166539 の反応式
Cl[CH:2]([C:8]1[CH:13]=[CH:12][C:11]([CH3:14])=[C:10]([CH3:15])[CH:9]=1)[C:3](OCC)=[O:4].[NH2:16][C:17](N)=[S:18].Cl.[OH2:21]>C(OCCO)C>[CH3:15][C:10]1[CH:9]=[C:8]([CH:2]2[S:18][C:17](=[O:21])[NH:16][C:3]2=[O:4])[CH:13]=[CH:12][C:11]=1[CH3:14]
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 962WaterHCID 2723790ThioureaHCID 10799298Ethyl 2-chloro-2-(3,4-dimethylphenyl)acetate

生成物 1

HCID 12810954HCID 12810954、化合物収率 60%

試薬・触媒・溶媒 1

HCID 8076Glycol monoethyl ether溶媒

実験手順

2.26 g of ethyl α-chloro-α-(3,4-dimethylphenyl)acetate and 910 mg of thiourea, in 15 ml of ethylene glycol monoethyl ether, are stirred under reflux for 2 hours. Then, 1 ml of concentrated HCl is added and the mixture is further heated under reflux for 3.5 hours. After cooling, water is added and extraction is carried out with ethyl acetate. The extract is washed with water and dried (MgSO4). After the solvent is distilled off, column chromatography is carried out on the oily residue with 100 g of silica gel. The eluate with chloroform-ethyl acetate (5:1) yields crystals of 5-(3,4-dimethylphenyl)thiazolidine-2,4-dione 1.32 g (60%). Recrystallization from cyclohexane-ethyl acetate gives colorless prisms, m.p. 121°-122° C.

後処理

  1. temperatureunder reflux for 2 hours
  2. temperaturethe mixture is further heated
  3. temperatureunder reflux for 3.5 hours
  4. temperatureAfter cooling
  5. extractionextraction
  6. washThe extract is washed with water
  7. dry with materialdried (MgSO4)
  8. distillationAfter the solvent is distilled off

出典と根拠

ORDレコード
ord-565dcff0765548df9891ad7756aad189
出典データセット
uspto-grants-1983_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04387101

反応ノート

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