Dimethyl Sulfate → HCID 21835795、化合物

HRID 1586551ノート

反応式

HRID 1586551 の反応式
[C:1]([CH:4]=[N:5][C:6]1[C:7](=[CH:11][CH:12]=[C:13]([Cl:15])[CH:14]=1)[C:8](O)=[O:9])([OH:3])=[O:2].[C:16](=O)([O-])[O-].[K+].[K+].S([O:27][CH3:28])(OC)(=O)=O>CN(C)C=O>[C:1]([CH:4]=[N:5][C:6]1[C:7](=[CH:11][CH:12]=[C:13]([Cl:15])[CH:14]=1)[C:8]([O:27][CH3:28])=[O:9])([O:3][CH3:16])=[O:2]

参加物

5

反応物 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 19597249HCID 19597249、化合物

生成物 1

HCID 21835795HCID 21835795、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

17 g (66 mmol) of N-carboxymethylene-4-chloroanthranilic acid are dissolved in 175 g of N,N-dimethylformamide, and 22.5 g (162 mmol) of potassium carbonate are added. At 80° C., 56 g (444 mmol) of dimethyl sulfate are added dropwise in 3 portions over the course of 2 h, and the mixture is then stirred for 30 min. The excess dimethyl sulfate is destroyed by adding ammonia. The product is precipitated by cooling, filtered off and washed with water. 16.1 g (62.5 mmol; 95%) of methyl N-carbomethoxymethylene-4-chloroanthranilate are isolated.

後処理

  1. customThe excess dimethyl sulfate is destroyed
  2. additionby adding ammonia
  3. customThe product is precipitated
  4. temperatureby cooling
  5. filtrationfiltered off
  6. washwashed with water

出典と根拠

ORDレコード
ord-1a377c485efd47a19c9ed3abf55a3c32
出典データセット
uspto-grants-1999_08
特許番号
US05945556

反応ノート

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