Hydrochloric Acid → HCID 11185063, 화합물

HRID 1680831노트

반응식

HRID 1680831 반응식
[NH2:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[C:7]([CH3:17])[C:3]=1[C:4]([OH:6])=[O:5].N1C=CC=CC=1.[C:24](Cl)(=[O:26])[CH3:25].Cl>C1C=CC=CC=1>[C:24]([NH:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[C:7]([CH3:17])[C:3]=1[C:4]([OH:6])=[O:5])(=[O:26])[CH3:25]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6367Acetyl chlorideHCID 126858402-Amino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid

생성물 1

HCID 11185063HCID 11185063, 화합물수율 86.6%

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

To a mixture consisting of 1 g of 2-amino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid, 20 ml of benzene, and 0.7 ml of pyridine in a flask cooled with ice water was added dropwise with stirring a solution of 600 mg of acetyl chloride in 5 ml of benzene. The mixture was further stirred for 5 hours at room temperature, and then heated to reflux for one hour. After cooling, the mixture was shaken with dilute hydrochloric acid and the layers were separated. The acidic aqueous layer was extracted with ethyl acetate, and the combined organic extracts were washed with water, and dried over sodium sulfate. The solvent was removed by distillation. The resulting residue was recrystallized from ethanol/water to yield 1.02 g of 2-acetylamino-5-ethoxycarbonyl-4,6-dimethylbenzoic acid melting at 170°-171° C.

후처리

  1. additionwas added dropwise
  2. temperatureheated
  3. temperatureto reflux for one hour
  4. temperatureAfter cooling
  5. customthe layers were separated
  6. extractionThe acidic aqueous layer was extracted with ethyl acetate
  7. washthe combined organic extracts were washed with water
  8. dry with materialdried over sodium sulfate
  9. customThe solvent was removed by distillation
  10. customThe resulting residue was recrystallized from ethanol/water

출처 및 근거

ORD 기록
ord-93fbbec4f8b44f7f9073021acd3c7396
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04276295

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