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

HRID 1382758ノート

反応式

HRID 1382758 の反応式
[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]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 799823-ChloropropanamideHCID 3080818Tilnoprofenic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-af576c056a4f4b5e9b8c91f5fb1e8cc3
出典データセット
uspto-grants-1989_02
特許番号
US04808593

反応ノート

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