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Sodium Hydroxide → HCID 22258014、化合物

HRID 1251591
ノート
印刷プレビュー

反応式

HRID 1251591 の反応式
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[C:9]([S:23][C:24]3[CH:29]=[CH:28][C:27]([N+:30]([O-])=O)=[CH:26][CH:25]=3)=[C:10]([CH2:12][C:13]3[C:22]4[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=4)[CH:16]=[CH:15][CH:14]=3)[S:11][C:5]=2[N:4]([CH2:33][CH:34]([CH3:36])[CH3:35])[C:3]1=[O:37].[Cl-].[NH4+].[OH-].[Na+]>C(O)C.O.[Fe]>[NH2:30][C:27]1[CH:28]=[CH:29][C:24]([S:23][C:9]2[C:6]3[C:7](=[O:8])[N:2]([CH3:1])[C:3](=[O:37])[N:4]([CH2:33][CH:34]([CH3:36])[CH3:35])[C:5]=3[S:11][C:10]=2[CH2:12][C:13]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH:16]=[CH:15][CH:14]=2)=[CH:25][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 22257984HCID 22257984、化合物

生成物 1

HCID 22258014HCID 22258014、化合物収率 5.5%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒
HCID 962
Water
溶媒

実験手順

A suspension of the crude 3-methyl-1-(2-methylpropyl)-6-(1-naphthalenylmethyl)-5-[(4-nitrophenyl)thio]thieno[2,3-d]pyrimidine-2,4-(1H, 3H)-dione (Example 35, 1.26 g), iron powder (0.59 g) and ammonium chloride (0.56 g) in ethanol (5 ml) and water (5 ml) was heated at reflux for 4 hours, then cooled to room temperature. Sodium hydroxide solution (10%, 50 ml) was added and the mixture was stirred for 1 hour. The resulting solution was decanted from insoluble solid. The solid and solution were in turn extracted with dichloromethane (3×50 ml) then ethyl acetate (3×50 ml). The combined organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was partially purified by column chromatography over silica, eluting with ethyl acetate:isohexane (1:1). Some pure material was recrystallised from isohexane: ethyl acetate to give the title compound (0.065 g). The remaining material was purified by preparative normal-phase HPLC with dichloromethane:ethanol gradient elution to give the title compound (0.163 g).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 4 hours
  3. customThe resulting solution was decanted from insoluble solid
  4. extractionextracted with dichloromethane (3×50 ml)
  5. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customThe residue was partially purified by column chromatography over silica
  9. washeluting with ethyl acetate:isohexane (1:1)
  10. customSome pure material was recrystallised from isohexane

出典と根拠

ORDレコード
ord-4ab24c6258f845a392f500726e4e3e3a
出典データセット
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06342502B1

反応ノート

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