Hydrochloric Acid → 2-Acetyl-2-methylpropane-1,3-diol bismethanesulphonate

HRID 2286763ノート

反応式

HRID 2286763 の反応式
[O:1]=[C:2]([CH3:9])[C:3]([CH2:7][OH:8])([CH2:5][OH:6])[CH3:4].[CH3:10][S:11](Cl)(=[O:13])=[O:12].N1C=CC=CC=1.Cl>ClCCCl>[CH3:10][S:11]([O:6][CH2:5][C:3]([C:2](=[O:1])[CH3:9])([CH3:4])[CH2:7][O:8][S:11]([CH3:10])(=[O:13])=[O:12])(=[O:13])=[O:12]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 5365163,3-Bis(hydroxymethyl)-2-butanone

生成物 1

HCID 47373912-Acetyl-2-methylpropane-1,3-diol bismethanesulphonate収率 70%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

66 g (0.5 mol) of 3-oxo-2,2-bis-[hydroxymethyl]-butane (for the preparation, see Beilstein H 1, E III 3306, IV 4132 and J. Chem. Soc., London 1932, 2671) were dissolved in 300 ml of 1,2-dichloroethane, 114.5 g (1 mol) of methanesulphonyl chloride were added dropwise and 158 g (2 mol) of pyridine were added dropwise at 0° to 5° C. The reaction mixture was stirred for a further 15 hours at room temperature and the batch was then introduced into 600 ml of ice-water and 100 ml of concentrated hydrochloric acid. A solid precipitated out and this was filtered off. The aqueous phase was extracted with 1 liter of methylene chloride; the solid was dissolved in the methylene chloride phase, the organic phase was dried over sodium sulphate, the solvent was distilled off under a waterpump vacuum and the residue was suspended in 200 ml of ether. 100 g (about 70% of theory) of 2-acetyl-2-methyl-propane-1,3-diol bismethanesulphonate with a melting point of 105° to 108° C. were obtained. ##STR12##

後処理

  1. customA solid precipitated out
  2. filtrationthis was filtered off
  3. extractionThe aqueous phase was extracted with 1 liter of methylene chloride
  4. dissolutionthe solid was dissolved in the methylene chloride phase
  5. dry with materialthe organic phase was dried over sodium sulphate
  6. distillationthe solvent was distilled off under a waterpump vacuum

出典と根拠

ORDレコード
ord-7a8f1e7b753a43529a089dfd80bb4499
出典データセット
uspto-grants-1981_05
特許番号
US04267381

反応ノート

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