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

HRID 335415노트

반응식

HRID 335415 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-ed2c98c3c70d41789dd13c2915c94d12
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08884010B2

반응 노트

불러오는 중…