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Phenylacetonitrile → HCID 20520018, 화합물

HRID 436260
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HRID 436260 반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([Cl:11])[N:3]=1.[CH2:12]([C:19]#[N:20])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[H-].[Na+]>O1CCOCC1>[C:19]([CH:12]([C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4]([Cl:11])[N:3]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)#[N:20]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8794PhenylacetonitrileHCID 24758Sodium hydrideHCID 852392,6-Dichloro-3-nitropyridine

생성물 1

HCID 20520018HCID 20520018, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
30 °C

실험 절차

There were gradually added to a cooled and stirred solution of 190 grams of 2,6-dichloro-3-nitropyridine and 117 grams of benzyl cyanide in 2 liters of dioxane under a nitrogen atmosphere 64 grams of sodium hydride (80% in white oil). The reaction mixture immediately turned a deep dark blue color, gradually a finely divided precipitate began to separate out, the temperature rose (with cooling with ice water) to 30° C. After 3 hours the mixture was treated with about 20 ml of ethyl alcohol, stirred for another 20 minutes, then filtered with suction. The deep blue sodium salt was dissolved in 1 liter of water, treated with dilute acetic acid until the color changed. The 2-(α-cyanobenzyl)-3-nitro-6-chloropyridine formed crystallized out in pure form. M.P. 165° C; Yield 146 grams.

후처리

  1. additionThere were gradually added to
  2. temperaturea cooled
  3. customto separate out
  4. additionAfter 3 hours the mixture was treated with about 20 ml of ethyl alcohol
  5. filtrationfiltered with suction
  6. dissolutionThe deep blue sodium salt was dissolved in 1 liter of water
  7. additiontreated with dilute acetic acid until the color

출처 및 근거

ORD 기록
ord-bdb3fde70ab64ca1ab0406495338c9e6
출처 데이터셋
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04008223

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