4-Toluenesulfonyl chloride → 5-(3-Acetyl-2,4,6-trimethylphenyl)-2-[1-(ethoxyimino)butyl]-3-(4-toluenesulfonyl)oxy-cyclohex-2-en-1-one

HRID 978992ノート

反応式

HRID 978992 の反応式
[Na].[C:2]([C:5]1[C:6]([CH3:29])=[C:7]([CH:13]2[CH2:18][C:17](=[O:19])[C:16]([C:20](=[N:24][O:25][CH2:26][CH3:27])[CH2:21][CH2:22][CH3:23])=[C:15]([OH:28])[CH2:14]2)[C:8]([CH3:12])=[CH:9][C:10]=1[CH3:11])(=[O:4])[CH3:3].[C:30]1([CH3:40])[CH:35]=[CH:34][C:33]([S:36](Cl)(=[O:38])=[O:37])=[CH:32][CH:31]=1>CC(C)=O>[C:2]([C:5]1[C:6]([CH3:29])=[C:7]([CH:13]2[CH2:14][C:15](=[O:28])[C:16]([C:20](=[N:24][O:25][CH2:26][CH3:27])[CH2:21][CH2:22][CH3:23])=[C:17]([O:19][S:36]([C:33]3[CH:34]=[CH:35][C:30]([CH3:40])=[CH:31][CH:32]=3)(=[O:38])=[O:37])[CH2:18]2)[C:8]([CH3:12])=[CH:9][C:10]=1[CH3:11])(=[O:4])[CH3:3]

参加物

5

反応物 3

HCID 73974-Toluenesulfonyl chlorideHCID 5360545SodiumHCID 136058378HCID 136058378、化合物

生成物 1

HCID 867415245-(3-Acetyl-2,4,6-trimethylphenyl)-2-[1-(ethoxyimino)butyl]-3-(4-toluenesulfonyl)oxy-cyclohex-2-en-1-one収率 95.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

The sodium salt of 5-(3-acetyl-2,4,6-trimethylphenyl)-2-[1-(ethoxyimino)butyl]-3-hydroxy-cyclohex-2-en-1-one (0.10 g; 0.26 mmole) was dissolved in acetone and then 4-toluenesulfonyl chloride (0.05 g; 0.26 mmole) was added. The mixture was stirred for 15 minutes and then the solvent was removed by evaporation under reduced pressure using a rotary evaporator. The product was purified by column chromatography over silica gel (eluant dichloromethane) to give 5-(3-acetyl-2,4,6-trimethylphenyl)-2-[1-(ethoxyimino)butyl]-3-(4-toluenesulfonyl)oxy-cyclohex-2-en-1-one (0.13 g; 95.6%) as a yellow oil.

後処理

  1. customthe solvent was removed by evaporation under reduced pressure
  2. customa rotary evaporator
  3. customThe product was purified by column chromatography over silica gel (eluant dichloromethane)

出典と根拠

ORDレコード
ord-cc4fef3e2230476087e7179769de5c4b
出典データセット
uspto-grants-1987_05
特許番号
US04666510

反応ノート

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