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Potassium Cyanide → HCID 70817665, 화합물

HRID 1753096
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HRID 1753096 반응식
Cl[CH2:2][C:3]1[CH:4]=[N:5][N:6]([CH:12]([CH3:14])[CH3:13])[C:7]=1[C:8]([F:11])([F:10])[F:9].[C-:15]#[N:16].[K+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O1CCOCC1.O.CCOC(C)=O>[CH:12]([N:6]1[C:7]([C:8]([F:11])([F:10])[F:9])=[C:3]([CH2:2][C:15]#[N:16])[CH:4]=[N:5]1)([CH3:14])[CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 9032Potassium CyanideHCID 664366344-(chloromethyl)-1-isopropyl-5-(trifluoromethyl)-1H-pyrazole

생성물 1

HCID 70817665HCID 70817665, 화합물수율 104%

시약·촉매·용매 4

HCID 74236Tetrabutylammonium Bromide촉매HCID 962Water용매HCID 8857Ethyl Acetate
용매
HCID 312751,4-Dioxane용매

실험 절차

Tetrabutyl ammonium bromide (7.95 gm, 24.7 mmol) was added to 4-(chloromethyl)-1-isopropyl-5-(trifluoromethyl)-1H-pyrazole (7 g, 31 mmol) in dioxane (75 mL) and water (75 mL) and the mixture was stirred for 10 minutes. Potassium cyanide (7.42 g, 114 mmol) was added and the mixture was stirred for 16 hours at room temperature. The mixture was diluted with EtOAc (100 mL) then the organic phase was washed with water (100 mL), brine (100 mL) and dried over sodium sulphate. The filtrate was evaporated in vacuo and purified by silica gel column chromatography eluting with hexane:EtOAc 90:10 to afford the title compound as a white solid (100%, 7.00 g).

후처리

  1. stirringthe mixture was stirred for 16 hours at room temperature
  2. washthe organic phase was washed with water (100 mL), brine (100 mL)
  3. dry with materialdried over sodium sulphate
  4. customThe filtrate was evaporated in vacuo
  5. custompurified by silica gel column chromatography
  6. washeluting with hexane:EtOAc 90:10

출처 및 근거

ORD 기록
ord-a6597770d8464096a619b0b7f0e44c97
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09163021B2

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