Hydrochloric Acid → 2-[1-(3-Chloroallyloxyimino)propyl]-3-hydroxy-5-(4-methanesulfonamidophenyl)-2-cyclohexen-1-one

HRID 2164362ノート

反応式

HRID 2164362 の反応式
C(O)C.C(Cl)(Cl)Cl.[OH:8][C:9]1[CH2:14][CH:13]([C:15]2[CH:20]=[CH:19][C:18]([NH:21][S:22]([CH3:25])(=[O:24])=[O:23])=[CH:17][CH:16]=2)[CH2:12][C:11](=[O:26])[C:10]=1[C:27](=O)[CH2:28][CH3:29].[Cl:31][CH:32]=[CH:33][CH2:34][O:35][NH2:36].Cl>C(O)C>[Cl:31][CH:32]=[CH:33][CH2:34][O:35][N:36]=[C:27]([C:10]1[C:11](=[O:26])[CH2:12][CH:13]([C:15]2[CH:16]=[CH:17][C:18]([NH:21][S:22]([CH3:25])(=[O:23])=[O:24])=[CH:19][CH:20]=2)[CH2:14][C:9]=1[OH:8])[CH2:28][CH3:29]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3036833O-(3-Chloroallyl)hydroxylamineHCID 21889567Chloroform ethanolHCID 178458872HCID 178458872、化合物

生成物 1

HCID 1361187982-[1-(3-Chloroallyloxyimino)propyl]-3-hydroxy-5-(4-methanesulfonamidophenyl)-2-cyclohexen-1-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Into 40 ml of mixture solvent of ethanol-chloroform (1:1) was dissolved 2 g of 3-hydroxy-5-(4-methanesulfonamidophenyl)-2-propionyl-2-cyclohexen-1-one and to the solution was added 10 ml of ethanol containing 10% of 3-chloroallyloxyamine at room temperature. The mixture was kept for 3 hours and it was poured into ice water. The mixture was acidified with hydrochloric acid and the oil separated was extracted with chloroform. The chloroform solution was dried with anhydrous magnesium sulfate and the chloroform was removed from it under reduced pressure and 1.5 g of the desired crude compound was obtained. It was purified by column chromatography and trans-cis mixture which was pale pink crystal having a melting point of 125°-127° C. was obtained.

後処理

  1. customthe oil separated
  2. extractionwas extracted with chloroform
  3. dry with materialThe chloroform solution was dried with anhydrous magnesium sulfate
  4. customthe chloroform was removed from it under reduced pressure

出典と根拠

ORDレコード
ord-b4e129651a044f9ead918991184d0033
出典データセット
uspto-grants-1985_03
特許番号
US04504305

反応ノート

読み込み中…