Water → HCID 178489010、化合物

HRID 1587407ノート

反応式

HRID 1587407 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178489010HCID 178489010、化合物収率 53.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d09103a12bc443c9b1552e7355d49de0
出典データセット
uspto-grants-1993_06
特許番号
US05217971

反応ノート

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