Hydrochloric Acid → 3,5-Dimethyl-4-nitrosophenol

HRID 1153999

반응식

HRID 1153999 반응식
Cl.[CH3:2][C:3]1[CH:4]=[C:5]([OH:10])[CH:6]=[C:7]([CH3:9])[CH:8]=1.[N:11]([O-])=[O:12].[Na+]>C(O)C.O>[CH3:2][C:3]1[CH:4]=[C:5]([OH:10])[CH:6]=[C:7]([CH3:9])[C:8]=1[N:11]=[O:12]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 79483,5-DimethylphenolHCID 23668193Sodium Nitrite

생성물 1

HCID 2360193,5-Dimethyl-4-nitrosophenol수율 71.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

750 ml of concentrated HCl are added to a solution of 3,5-dimethyl phenol (80.6 g) in 750 ml of 95% ethyl alcohol. The mixture is cooled to 0° C. in an ice/methanol bath. While maintaining the temperature of the reaction mixture below 5° C., a solution of NaNO2 (69.0 g) in 150 ml of H2O is added dropwise to the reaction mixture. The mixture is stirred at 0° C. for more than an hour and then poured into 9 liters of water. The aqueous mixture is filtered to give a yellow solid which is recrystallized from hot methanol and filtered to give 71.45 grams of a yellow solid, M.P. 180°-181° C. (dec.).

후처리

  1. temperatureWhile maintaining the temperature of the reaction mixture below 5° C.
  2. filtrationThe aqueous mixture is filtered
  3. customto give a yellow solid which
  4. customis recrystallized from hot methanol
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-f82a4ff692a44bb28cec908713f07b42
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487779

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