1-Benzyl-2-(1-methylsulfonyl-2-propylidene)hydrazine monohydrochloride → 1-Benzyl-2-(1-methylsulfonyl-2-propylidene)hydrazine

HRID 335415ノート

反応式

HRID 335415 の反応式
Cl.[CH2:2]([NH:9][N:10]=[C:11]([CH3:17])[CH2:12][S:13]([CH3:16])(=[O:15])=[O:14])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>C(=O)([O-])O.[Na+]>[CH2:2]([NH:9][N:10]=[C:11]([CH3:17])[CH2:12][S:13]([CH3:16])(=[O:14])=[O:15])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

参加物

3

反応物 1

HCID 866893461-Benzyl-2-(1-methylsulfonyl-2-propylidene)hydrazine monohydrochloride

生成物 1

HCID 866893471-Benzyl-2-(1-methylsulfonyl-2-propylidene)hydrazine収率 90.5%

試薬・触媒・溶媒 1

HCID 516892Sodium Bicarbonate溶媒

実験手順

To a 50 ml volume three-necked flask, 1-methylsulfonyl-2-propanone (7-2-1) (2.01 g), methanol (10 ml) and benzylhydrazine monohydrochloride (14-c) (2.56 g) were added under a nitrogen atmosphere at room temperature, then additional methanol (10 ml) was added. The resulting reaction mixture was stirred at room temperature for three days, and filtered to give the primary crystal. The filtrate was concentrated under reduced pressure, and filtered again to give the crystal. The crystal was combined with the primary crystal to give 4.2 g of 1-benzyl-2-(1-methylsulfonyl-2-propylidene)hydrazine monohydrochloride (5-2-3). Additionally, the hydrochloride (5-2-3) (0.28 g) was dissolved in saturated aqueous sodium hydrogen carbonate solution (5.0 ml), and extracted with tert-butyl methyl ether (5.0 ml) 2 times. Then, the organic layer was concentrated under reduced pressure to give 0.22 g of 1-benzyl-2-(1-methylsulfonyl-2-propylidene)hydrazine (5-2-3′). NMR data of Compound (5-2-3′) is shown below.

後処理

  1. extractionextracted with tert-butyl methyl ether (5.0 ml) 2 times
  2. concentrationThen, the organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-ed2c98c3c70d41789dd13c2915c94d12
出典データセット
uspto-grants-2014_11
特許番号
US08884010B2

反応ノート

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