Acetic Anhydride → 5-[(2-Methoxyphenyl)methylene]-2-thioxo-4-imidazolidinone

HRID 1464644노트

반응식

HRID 1464644 반응식
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH:5]=O.[NH:11]1[CH2:17][C:15](=[O:16])[NH:14][C:12]1=[S:13].C([O-])(=O)C.[Na+].C(OC(=O)C)(=O)C>O.C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH:5]=[C:17]1[NH:11][C:12](=[S:13])[NH:14][C:15]1=[O:16]

참가 물질

7

반응물 4

HCID 7918Acetic AnhydrideHCID 86582-MethoxybenzaldehydeHCID 517045Sodium AcetateHCID 12740302-Thiohydantoin

생성물 1

HCID 30046725-[(2-Methoxyphenyl)methylene]-2-thioxo-4-imidazolidinone수율 85.4%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

A mixture of 2-methoxybenzaldehyde (2.5 g, 18 mmoles), 2-thiohydantoin (2.0 g, 17 mmoles), sodium acetate (4.0 g, 49 mmoles), acetic anhydride (1/2 ml), and acetic acid (15 ml) is stirred under an inert atmosphere and heated to reflux. After 1 hour the mixture is stirred into water (300 ml), and the precipitate is filtered off, rinsed with water three times and dried. The product is triturated in boiling methanol, filtered off, and dried to afford the pure product (3.4 g), mp 234°-235° C.

후처리

  1. temperatureheated to reflux
  2. filtrationthe precipitate is filtered off
  3. washrinsed with water three times
  4. customdried
  5. customThe product is triturated
  6. filtrationfiltered off
  7. customdried

출처 및 근거

ORD 기록
ord-6f39e274d08449ee91317a0c9fed822a
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05306822

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