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

HRID 579229노트

반응식

HRID 579229 반응식
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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-1e7f7a7d63024a66a65a67f4f9415fb7
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040709B2

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