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Potassium Cyanide → HCID 70817665、化合物

HRID 82227
ノート
印刷プレビュー

反応式

HRID 82227 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 100%

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 min. 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 column chromatography on silica gel (hexane:EtOAc 90:10) to afford the title compound as a white solid in 100% yield, 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 column chromatography on silica gel (hexane:EtOAc 90:10)

出典と根拠

ORDレコード
ord-2cc2460879b54b2b848eb5727a989389
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846698B2

反応ノート

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