Sulfuric Acid → HCID 21714399, 화합물

HRID 650107

반응식

HRID 650107 반응식
[C:1]([C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[OH:10])#[N:2].[N+:11]([O-])([O-:13])=[O:12].[Na+].S(=O)(=O)(O)O.N([O-])=O.[Na+]>C(Cl)Cl>[N+:11]([C:5]1[CH:6]=[CH:7][C:8]([Cl:9])=[C:3]([C:1]#[N:2])[C:4]=1[OH:10])([O-:13])=[O:12]

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 24268Sodium NitrateHCID 44079952-Chloro-6-hydroxybenzonitrileHCID 23668193Sodium Nitrite

생성물 1

HCID 21714399HCID 21714399, 화합물수율 29.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

2-cyano-3-chlorophenol(2.8 g, 18.3 mmol) was dissolved in methylene chloride(40 ml) followed by the addition of sodium nitrate (1.70 g, 20.1 mmol). The addition of sulfuric acid (15 ml/ 3M) is then made, followed by addition of a catalytic amount of sodium nitrite. The mixture is allowed to stir. After 24 hrs, the reaction mixture is diluted with methylene chloride and extracted with water. The organic layer is dried over MgSO4 and filtered. The solvent was evaporated and chromatography of the resulting solid on silica gel (4%MeOH/CH2Cl2) gave the desired product(1.05 g, 29.2%). 1H NMR (CD3COCD3): δ8.09 (d,1H), 6.55 (d, 1H).

후처리

  1. extractionextracted with water
  2. dry with materialThe organic layer is dried over MgSO4
  3. filtrationfiltered
  4. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-b4e57e296ab54723b9453373aa2395f6
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06271261B1

연결된 노트

불러오는 중…