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

HRID 917404
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인쇄 미리보기

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HRID 917404 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-c50415224a2f482d976daa0add79a524
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07273878B2

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