Water → HCID 178489010, 화합물

HRID 1587407노트

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HRID 1587407 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=O)[CH:10]([C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)Cl)=[CH:5][CH:4]=1.[NH2:21][C:22]([NH2:27])=[N:23][C:24]([NH2:26])=[S:25].O>C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:26]=[C:24]([NH:23][C:22]([NH2:27])=[NH:21])[S:25][C:10]=2[C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 2724563AmidinothioureaHCID 38625232-Chloro-1,2-bis(4-methoxyphenyl)ethan-1-one

생성물 1

HCID 178489010HCID 178489010, 화합물수율 53.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1,2-bis(4-methoxyphenyl)-2-chloroethanone (1.00 g) and N-diaminomethylenethiourea (0.65 g) in ethanol (20 ml) was refluxed for 12 hours. After allowing to cool to ambient temperature, then the reaction mixture was poured into water and extracted with ethyl acetate. The separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed n alumina, eluting with a mixture of chloroform and methanol. The desired fractions were combined and concentrated in vacuo. The residue was washed with isopropy ether to give 4,5-bis(4methoxyphenyl)-2-guanidinothiazole (0.65 g).

후처리

  1. temperaturewas refluxed for 12 hours
  2. extractionextracted with ethyl acetate
  3. washThe separated organic layer was washed with water and brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was chromatographed n alumina
  7. washeluting with a mixture of chloroform and methanol
  8. concentrationconcentrated in vacuo
  9. washThe residue was washed with isopropy ether

출처 및 근거

ORD 기록
ord-d09103a12bc443c9b1552e7355d49de0
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05217971

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