Potassium Carbonate → HCID 21958890、化合物

HRID 2213858ノート

反応式

HRID 2213858 の反応式
Cl[CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1.[C:11]([O:22][CH2:23][CH3:24])(=[O:21])[C:12]1[CH:20]=[CH:19][C:17]([OH:18])=[C:14]([O:15][CH3:16])[CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:16][O:15][C:14]1[CH:13]=[C:12]([CH:20]=[CH:19][C:17]=1[O:18][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)[C:11]([O:22][CH2:23][CH3:24])=[O:21]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12038Ethyl vanillateHCID 958344-(3-Chloropropyl)morpholine

生成物 1

HCID 21958890HCID 21958890、化合物収率 100%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

N-(3-Chloropropyl)morpholine (90 g, 0.55 mol) was added dropwise, over 30 minutes, to a solution of ethyl vanillate (98 g, 0.50 mol) and powdered potassium carbonate (104 g, 0.75 mol) in dimethylformamide (300 ml) at 80° C. The reaction was heated at 80° C. for 90 minutes, cooled to ambient temperature, filtered and the filtrate concentrated in vacuo. The crude product was taken up in diethyl ether (1000 ml), filtered and washed with water (2×200 ml) and brine (200 ml). Solvent evaporation in vacuo yielded ethyl 3-methoxy-4-(3-morpholinopropoxy)benzoate (161.5 g, 100% yield) as a pale yellow oil which crystallised on standing to afford a pale yellow solid:

後処理

  1. temperaturecooled to ambient temperature
  2. filtrationfiltered
  3. concentrationthe filtrate concentrated in vacuo
  4. filtrationfiltered
  5. washwashed with water (2×200 ml) and brine (200 ml)
  6. customSolvent evaporation in vacuo

出典と根拠

ORDレコード
ord-19c4b39d2c7b4921b7e2e178451a0324
出典データセット
uspto-grants-2006_09
特許番号
US07105669B1

反応ノート

読み込み中…