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Potassium Carbonate → HCID 21842452、化合物

HRID 1737240
ノート
印刷プレビュー

反応式

HRID 1737240 の反応式
Cl.Cl.[NH2:3][C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:11]=2[Cl:17])[N:7]=[C:6]([N:18]2[CH2:22][CH2:21][CH:20]([CH2:23][NH2:24])[CH2:19]2)[N:5]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:31][S:32](Cl)(=[O:34])=[O:33]>C1COCC1>[ClH:16].[NH2:3][C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:11]=2[Cl:17])[N:7]=[C:6]([N:18]2[CH2:22][CH2:21][CH:20]([CH2:23][NH:24][S:32]([CH3:31])(=[O:34])=[O:33])[CH2:19]2)[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 21842411HCID 21842411、化合物

生成物 1

HCID 21842452HCID 21842452、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In 40 ml of THF was dissolved 2.1 g of the free base obtained by neutralizing the compound of Example 62, followed by addition of 0.94 g of potassium carbonate and 0.78 g of methanesulfonyl chloride. The mixture was reacted at room temperature for 20 hours. The THF was removed by concentration and the residue was diluted with water and extracted with chloroform. The extract was washed with water and dried and the chloroform was distilled off. The residue was purified by silica gel column chromatography (elution with CHCl3 :MeOH=19:1) and the resulting oil, 2.3 g, was treated in the same manner as in Example 32 (Step 2) to provide the title compound. m.p. 220-230° C.

後処理

  1. customobtained
  2. customThe mixture was reacted at room temperature for 20 hours
  3. customThe THF was removed by concentration
  4. additionthe residue was diluted with water
  5. extractionextracted with chloroform
  6. washThe extract was washed with water
  7. customdried
  8. distillationthe chloroform was distilled off
  9. customThe residue was purified by silica gel column chromatography (elution with CHCl3 :MeOH=19:1)
  10. additionthe resulting oil, 2.3 g, was treated in the same manner as in Example 32 (Step 2)

出典と根拠

ORDレコード
ord-2fba83cf48c64044bff02078ca9c4e09
出典データセット
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05962453

反応ノート

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