Dimethyl Sulfate → HCID 21835795, 화합물

HRID 1586551노트

반응식

HRID 1586551 반응식
[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]

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 19597249HCID 19597249, 화합물

생성물 1

HCID 21835795HCID 21835795, 화합물수율 95%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1a377c485efd47a19c9ed3abf55a3c32
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05945556

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