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Dimethylformamide → 6,6-difluoro-5-methyl-5-hexenyl N,N-dimethyldithiocarbamate

HRID 917404
ノート
印刷プレビュー

反応式

HRID 917404 の反応式
CN(C)C=O.CS(O[CH2:11][CH2:12][CH2:13][CH2:14][C:15]([CH3:19])=[C:16]([F:18])[F:17])(=O)=O.O.O.[CH3:22][N:23]([CH3:27])[C:24](=[S:26])[S-:25].[Na+]>O>[CH3:22][N:23]([CH3:27])[C:24](=[S:25])[S:26][CH2:11][CH2:12][CH2:13][CH2:14][C:15]([CH3:19])=[C:16]([F:17])[F:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 230203716,6-Difluoro-5-methyl-5-hexenyl methanesulfonateHCID 23693613Sodium dimethyldithiocarbamate dihydrate

生成物 1

HCID 230202846,6-difluoro-5-methyl-5-hexenyl N,N-dimethyldithiocarbamate収率 51.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

To 100 ml of N,N-dimethylformamide, 4.56 g (20 mmol) of 6,6-difluoro-5-methyl-5-hexenyl methanesulfonate and 4.70 g (26 mmol) of sodium dimethyldithiocarbamate dihydrate were dissolved, followed by stirring at 100° C. for 3 hours. The reaction liquid was poured into water and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentrating under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:10) to obtain 2.60 g (yield: 51%) of 6,6-difluoro-5-methyl-5-hexenyl N,N-dimethyldithiocarbamate.

後処理

  1. customThe reaction liquid
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialby drying over anhydrous magnesium sulfate
  5. concentrationconcentrating under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:10)

出典と根拠

ORDレコード
ord-c50415224a2f482d976daa0add79a524
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07273878B2

反応ノート

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