Ethanol → HCID 12832643、化合物

HRID 703246ノート

反応式

HRID 703246 の反応式
[C:1]([NH:4][C:5]([C:7]([NH:9][C:10](=O)[CH3:11])=[O:8])=[O:6])(=O)[CH3:2].N1[CH:18]=[CH:17][CH:16]=CC=1.O.[CH:20](Cl)(Cl)Cl.[CH2:24](O)[CH3:25]>>[C:7]([N:9]1[CH2:16][CH2:17][CH2:18][CH2:11][CH2:10]1)(=[O:8])[C:5]([N:4]1[CH2:25][CH2:24][CH2:20][CH2:2][CH2:1]1)=[O:6]

参加物

6

反応物 5

HCID 702EthanolHCID 962WaterHCID 1049PyridineHCID 6212ChloroformHCID 3016168N,N'-Diacetyloxamide2 回

生成物 1

HCID 12832643HCID 12832643、化合物収率 39.2%

実験手順

A suspension of N,N'-diacetyloxamide (10 g, 0.058 mol) in ethyl alcohol (20 ml) is charged into a three-necked flask equipped with a reflux condenser, an inlet tube for nitrogen, a dropping funnel, and a magnetic stirrer. 98 % Pyridine (40 ml, 0.40 mol) is then dripped therein at 70° C., and after 40 minutes the complete solving of N,N'-diacetyloxamide in the reaction mixture is observed. The temperature is brought to 95° C. and kept at this value for 6.5 hours. Then water (60 ml) and chloroform (60 ml) are added to the reaction mixture and the organic phase is separated. Chloroform is distilled off and ethyl ether (30 ml) is added to precipitate the compound of the title. The precipitate is recovered by filtration and dried, thus affording the compound of the title (5.1 g, 0.023 mol, yield 39.2%) with m.p. 88°-90° C.

後処理

  1. additionis charged into a three-necked flask
  2. customequipped with a reflux condenser, an inlet tube for nitrogen, a dropping funnel, and a magnetic stirrer
  3. customis brought to 95° C.
  4. customthe organic phase is separated
  5. distillationChloroform is distilled off
  6. additionethyl ether (30 ml) is added
  7. customto precipitate the compound of the title
  8. filtrationThe precipitate is recovered by filtration
  9. customdried
  10. customthus affording the compound of the title (5.1 g, 0.023 mol, yield 39.2%) with m.p. 88°-90° C.

出典と根拠

ORDレコード
ord-4d3599b3c7bd4f6f9a9e39fb515ac711
出典データセット
uspto-grants-1991_01
特許番号
US04981963

反応ノート

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