Hydrochloric Acid → Azidobenzene

HRID 2267128노트

반응식

HRID 2267128 반응식
Cl.[C:2]1([NH:8][NH2:9])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:10]([O-])=O.[Na+]>C(OCC)C.O>[C:2]1([N:8]=[N+:9]=[N-:10])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 7516PhenylhydrazineHCID 23668193Sodium Nitrite

생성물 1

HCID 69319Azidobenzene

시약·촉매·용매 2

HCID 962Water용매2회HCID 3283Diethyl Ether용매

실험 절차

Concentrated hydrochloric acid (20 ml) was cooled at 0° C. and a solution of 2.0 ml of phenylhydrazine in 7.0 ml of diethyl ether was dropped thereinto. After stirring for 10 minutes, a solution of 1.70 g of sodium nitrite dissolved in 2.0 ml of water was dropped thereinto and the mixture was stirred for 1 hour together with raising the temperature up to room temperature. Water was added to the reaction solution, the mixture was extracted with ethyl acetate and the ethyl acetate layer washed with a saturated saline solution and dried over sodium sulfate. The solvent was evaporated in vacuo to give 961 mg of the title compound as a red oily crude product.

후처리

  1. additionwas dropped
  2. stirringthe mixture was stirred for 1 hour together
  3. extractionthe mixture was extracted with ethyl acetate
  4. washthe ethyl acetate layer washed with a saturated saline solution
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-8e858540eb3e4ca78d1e2049c8699839
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858800B2

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