Methylhydrazine → 1-Methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine

HRID 335407ノート

反応式

HRID 335407 の反応式
[CH3:1][S:2]([CH2:5][C:6](=O)[CH3:7])(=[O:4])=[O:3].[CH3:9][NH:10][NH2:11]>C1(C)C=CC=CC=1>[CH3:9][NH:10][N:11]=[C:6]([CH3:7])[CH2:5][S:2]([CH3:1])(=[O:4])=[O:3]

参加物

4

反応物 2

HCID 6061Methylhydrazine2 回HCID 786951-(Methylsulphonyl)acetone

生成物 1

HCID 764689591-Methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine収率 59.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a 100 ml volume four-necked flask, 1-methylsulfonyl-2-propanone (7-2-1) (4.99 g) and toluene (36.0 g) were added under a nitrogen atmosphere, and added dropwise 40 wt % of aqueous monomethylhydrazine solution (14-a) (3.96 g) at room temperature. The resulting mixture was stirred at room temperature for 16 hours, and then added additional 40 wt % of aqueous monomethylhydrazine solution (0.35 g). The resulting mixture was stirred for 24 hours, and refluxed with Dean-Stark apparatus under reduced pressure at the internal temperature of 50° C. After refluxing, the resulting mixture was cooled to 0° C., and filtered to give 3.56 g of 1-methyl-2-(1-methylsulfonyl-2-propylidene)hydrazine (5-2-1).

後処理

  1. stirringThe resulting mixture was stirred for 24 hours
  2. temperaturerefluxed with Dean-Stark apparatus under reduced pressure at the internal temperature of 50° C
  3. temperatureAfter refluxing
  4. temperaturethe resulting mixture was cooled to 0° C.
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-094b7787433b4ec8bf7622d84c03d965
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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