Ethyl thiooxamate → Ethyl 4,5-bis(4-methoxyphenyl)thiazole-2-carboxylate

HRID 1587399노트

반응식

HRID 1587399 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](=[S:28])[C:23]([O:25][CH2:26][CH3:27])=[O:24]>C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:21]=[C:22]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[S:28][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

4

반응물 2

HCID 2733398Ethyl thiooxamateHCID 38625232-Chloro-1,2-bis(4-methoxyphenyl)ethan-1-one

생성물 1

HCID 10429180Ethyl 4,5-bis(4-methoxyphenyl)thiazole-2-carboxylate수율 96%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1,2-bis(4-methoxyphenyl)-2-chloroethanone (5.00 g) and ethyl 2-amino-2-thioxoacetate (3.44 g) in ethanol (30 ml) was refluxed for 4 hours. After allowing to cool to ambient temperature, the reaction mixture was filtered and washed with ethanol, and the filtrate was evaporated in vacuo. The residue was subjected to column chromatography on silica gel (300 g) and eluted with a mixture of hexane and ethyl acetate (8:1, V/V). The fractions containing the object compound were combined and concentrated under reduced pressure, and to give a oily compound of 4,5-bis(4-methoxyphenyl)-2-ethoxycarbonylthiazole (6.10 g).

후처리

  1. temperaturewas refluxed for 4 hours
  2. filtrationthe reaction mixture was filtered
  3. washwashed with ethanol
  4. customthe filtrate was evaporated in vacuo
  5. washeluted with a mixture of hexane and ethyl acetate (8:1, V/V)
  6. additionThe fractions containing the object compound
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7bf0920aec9b4d2dae712580e8258fc6
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05217971

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