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Hydrochloric Acid → HCID 12810954, 화합물

HRID 2166539
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HRID 2166539 반응식
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]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 2723790ThioureaHCID 10799298Ethyl 2-chloro-2-(3,4-dimethylphenyl)acetate

생성물 1

HCID 12810954HCID 12810954, 화합물수율 60%

시약·촉매·용매 1

HCID 8076Glycol monoethyl ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-565dcff0765548df9891ad7756aad189
출처 데이터셋
uspto-grants-1983_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04387101

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