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Potassium Cyanide → HCID 70817665、化合物

HRID 1753096
ノート
印刷プレビュー

反応式

HRID 1753096 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 2

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

生成物 1

HCID 70817665HCID 70817665、化合物収率 104%

試薬・触媒・溶媒 4

HCID 74236Tetrabutylammonium Bromide触媒HCID 962Water溶媒HCID 8857Ethyl Acetate
溶媒
HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a6597770d8464096a619b0b7f0e44c97
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09163021B2

反応ノート

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