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

HRID 579228ノート

反応式

HRID 579228 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

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. 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

出典と根拠

ORDレコード
ord-1c9f760c7b8744f6aac0a9cbbfe97638
出典データセット
uspto-grants-2015_05
特許番号
US09040709B2

反応ノート

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