Sulfuric Acid → HCID 21714399、化合物

HRID 650107ノート

反応式

HRID 650107 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 21714399HCID 21714399、化合物収率 29.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-b4e57e296ab54723b9453373aa2395f6
出典データセット
uspto-grants-2001_08
特許番号
US06271261B1

反応ノート

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