Potassium Carbonate → HCID 12138357、化合物

HRID 987182ノート

反応式

HRID 987182 の反応式
[SH:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([SH:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].[C:13]([C:17]1[CH:18]=[C:19]([CH:22]=[C:23]([C:25]([CH3:28])([CH3:27])[CH3:26])[CH:24]=1)[CH2:20]Br)([CH3:16])([CH3:15])[CH3:14].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[C:13]([C:17]1[CH:18]=[C:19]([CH:22]=[C:23]([C:25]([CH3:28])([CH3:27])[CH3:26])[CH:24]=1)[CH2:20][S:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([S:12][CH2:20][C:19]2[CH:18]=[C:17]([C:13]([CH3:15])([CH3:14])[CH3:16])[CH:24]=[C:23]([C:25]([CH3:28])([CH3:27])[CH3:26])[CH:22]=2)[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6])([CH3:16])([CH3:15])[CH3:14]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 44475071-(Bromomethyl)-3,5-di-tert-butylbenzeneHCID 12138349HCID 12138349、化合物

生成物 1

HCID 12138357HCID 12138357、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Methyl 3,5-dimercaptobenzoate (20.0 g, 100.0 mmol), 3,5-di-tertiarybutylbenzyl bromide (molecular weight 283.25, 57.0 g, 201.2 mmol) and potassium carbonate (molecular weight 138.21, 28.0 g, 202.6 mmol) were dissolved in 350 ml of acetone and the mixture was heated under reflux for 12 hours. The acetone and salts were removed, and the residue was purified by means of chromatography with dichloromethane as the developing solvent, giving methyl 3,5-bis(3,5-di-tertiary-butylbenzylthio)benzoate as needles.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 12 hours
  3. customThe acetone and salts were removed
  4. customthe residue was purified by means of chromatography with dichloromethane as the developing solvent

出典と根拠

ORDレコード
ord-73dc61c550854134852ef605f1144a32
出典データセット
uspto-grants-2003_10
特許番号
US06630578B2

反応ノート

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