2-Aminopyrimidine → HCID 20544711、化合物

HRID 2285506ノート

反応式

HRID 2285506 の反応式
[NH2:1][C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[Cl:8][C:9]1[CH:18]=[CH:17][C:12]2[O:13][CH2:14][CH2:15][O:16][C:11]=2[C:10]=1[C:19](Cl)=[O:20]>C(C(C)=O)C>[N:3]1[CH:4]=[CH:5][CH:6]=[N:7][C:2]=1[NH:1][C:19]([C:10]1[C:11]2[O:16][CH2:15][CH2:14][O:13][C:12]=2[CH:17]=[CH:18][C:9]=1[Cl:8])=[O:20]

参加物

4

反応物 2

HCID 79782-AminopyrimidineHCID 20544693HCID 20544693、化合物

生成物 1

HCID 20544711HCID 20544711、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
10 °C

実験手順

280 ml of methyl ethyl ketone, 13 g of 2-amino-pyrimidine were put into a 500 ml balloon flask provided with a stirrer and a thermometer. The mixture was cooled to 10° C. and 28 g of ground 6-chloro-1,4-benzodioxane-5-carbonyl chloride was added and stirred for two hours, the temperature being allowed to rise to 20° C. The obtained solid was filtered off, washed with 30 ml of methyl ethyl ketone and then dissolved in 250 ml of boiling water. The solution was treated with 10 ml of 36° Bel caustic soda lye. After filtration 12 g of product were obtained and crystallized again from 150 ml of ethanol. 9.5 g of N-(2-pyrimidyl)-6-chloro-1,4-benzodioxane-5-carboxamide was obtained. (M.P.: 223° C. with decomposition). The structure was confirmed by nuclear magnetic resonance analysis.

後処理

  1. customprovided with a stirrer
  2. customto rise to 20° C
  3. filtrationThe obtained solid was filtered off
  4. washwashed with 30 ml of methyl ethyl ketone
  5. dissolutiondissolved in 250 ml of boiling water
  6. additionThe solution was treated with 10 ml of 36° Bel caustic soda lye
  7. filtrationAfter filtration 12 g of product
  8. customwere obtained
  9. customcrystallized again from 150 ml of ethanol

出典と根拠

ORDレコード
ord-7d008ccd6a46465d99976d0215927d8b
出典データセット
uspto-grants-1982_04
特許番号
US04323503

反応ノート

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