Potassium Carbonate → 2-carbamoylethyl alpha,2-dimethyl-5H-[1]benzopyrano[2,3-b]pyridine7-acetate

HRID 1382758노트

반응식

HRID 1382758 반응식
[CH3:1][CH:2]([C:6]1[CH:7]=[CH:8][C:9]2[O:19][C:13]3=[N:14][C:15]([CH3:18])=[CH:16][CH:17]=[C:12]3[CH2:11][C:10]=2[CH:20]=1)[C:3]([OH:5])=[O:4].C(=O)([O-])[O-].[K+].[K+].Cl[CH2:28][CH2:29][C:30]([NH2:32])=[O:31]>CN(C)C=O>[CH3:1][CH:2]([C:6]1[CH:7]=[CH:8][C:9]2[O:19][C:13]3=[N:14][C:15]([CH3:18])=[CH:16][CH:17]=[C:12]3[CH2:11][C:10]=2[CH:20]=1)[C:3]([O:5][CH2:28][CH2:29][C:30](=[O:31])[NH2:32])=[O:4]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 799823-ChloropropanamideHCID 3080818Tilnoprofenic acid

생성물 1

HCID 143504562-carbamoylethyl alpha,2-dimethyl-5H-[1]benzopyrano[2,3-b]pyridine7-acetate수율 70.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

To a solution of 2.7 g of α,2-dimethyl-5H-[1]benzopyrano [2,3-b]pyridine-7-acetic acid in 15 ml of dimethylformamide are added 0.8 g of potassium carbonate and 1.3 g of 3-chloropropionamide, and stirred at 70° C. for 7.5 hours under a nitrogen atmosphere. The reaction mixture is poured into ice water. The precipitate is extracted with ethyl acetate, washed with water and dried, and then concentrated. The residue is recrystallized from ethanol to obtain 2.4 g of 2-carbamoylethyl α,2-dimethyl-5H-[1]benzopyrano[2,3-b]pyridine7-acetate as white crystals having a melting point of 143° to 145° C.

후처리

  1. extractionThe precipitate is extracted with ethyl acetate
  2. washwashed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue is recrystallized from ethanol

출처 및 근거

ORD 기록
ord-af576c056a4f4b5e9b8c91f5fb1e8cc3
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04808593

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