Selenium Dioxide → 5-Isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-formyl-2-morpholin-4-yl-pyrimidin-4-ylamide

HRID 356652ノート

反応式

HRID 356652 の反応式
[Cl:1][C:2]1[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][C:3]=1[O:4][C:5]1[C:6]([NH:18][S:19]([C:22]2[CH:27]=[CH:26][C:25]([CH:28]([CH3:30])[CH3:29])=[CH:24][N:23]=2)(=[O:21])=[O:20])=[N:7][C:8]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)=[N:9][C:10]=1[CH3:11].[Se](=O)=[O:38]>O1CCOCC1>[Cl:1][C:2]1[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][C:3]=1[O:4][C:5]1[C:6]([NH:18][S:19]([C:22]2[CH:27]=[CH:26][C:25]([CH:28]([CH3:30])[CH3:29])=[CH:24][N:23]=2)(=[O:21])=[O:20])=[N:7][C:8]([N:12]2[CH2:13][CH2:14][O:15][CH2:16][CH2:17]2)=[N:9][C:10]=1[CH:11]=[O:38]

参加物

4

反応物 2

HCID 24007Selenium DioxideHCID 223778355-Isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-methyl-2-morpholin-4-yl-pyrimidin-4-ylamide

生成物 1

HCID 223778605-Isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-formyl-2-morpholin-4-yl-pyrimidin-4-ylamide収率 51.6%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

1 g of the compound obtained in Example 36 and 2.1 g of selenium dioxide in 40 ml of dioxan were stirred in an autoclave at 170° C. for 7 hours. The reaction mixture was filtered and the filtrate was concentrated. The residue was partitioned between ethyl acetate and water. The organic phase was dried, the solvent was evaporated and the residue was purified over silica gel with ethyl acetate/hexane. 0.53 g of 5-isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-formyl-2-morpholin-4-yl-pyrimidin-4-ylamide, m.p. 194° C., was obtained.

後処理

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. customThe residue was partitioned between ethyl acetate and water
  4. customThe organic phase was dried
  5. customthe solvent was evaporated
  6. customthe residue was purified over silica gel with ethyl acetate/hexane

出典と根拠

ORDレコード
ord-c3b639ff2c404d589f278cae338f982e
出典データセット
uspto-grants-1998_11
特許番号
US05837708

反応ノート

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