Hydrazine, (phenylmethyl)-, hydrochloride (1:1) → 1-Benzyl-2-(1-methylsulfonyl-2-propylidene)hydrazine monohydrochloride

HRID 579228노트

반응식

HRID 579228 반응식
[CH3:1][S:2]([CH2:5][C:6](=O)[CH3:7])(=[O:4])=[O:3].[ClH:9].[CH2:10]([NH:17][NH2:18])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>CO>[ClH:9].[CH2:10]([NH:17][N:18]=[C:6]([CH3:7])[CH2:5][S:2]([CH3:1])(=[O:4])=[O:3])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

참가 물질

4

반응물 2

HCID 14084Hydrazine, (phenylmethyl)-, hydrochloride (1:1)HCID 786951-(Methylsulphonyl)acetone

생성물 1

HCID 866893461-Benzyl-2-(1-methylsulfonyl-2-propylidene)hydrazine monohydrochloride수율 102.8%

시약·촉매·용매 1

HCID 887Methanol용매2회

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. customThe resulting reaction mixture
  2. filtrationfiltered
  3. customto give the primary crystal
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. filtrationfiltered again
  6. customto give the crystal

출처 및 근거

ORD 기록
ord-1c9f760c7b8744f6aac0a9cbbfe97638
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040709B2

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