Hydrochloric Acid → N-(8-Amino-6-fluoro-5-methyl-1-oxo-1,2,3,4-tetrahydronaphthalen-2-yl)acetamide

HRID 1458312ノート

反応式

HRID 1458312 の反応式
[C:1]([NH:4][CH:5]1[CH2:14][CH2:13][C:12]2[C:7](=[C:8]([NH:17]C(=O)C)[CH:9]=[C:10]([F:16])[C:11]=2[CH3:15])[C:6]1=[O:21])(=[O:3])[CH3:2].Cl.C(=O)([O-])[O-].[K+].[K+].[O-][Si]([O-])=O.[Mg+2]>O>[C:1]([NH:4][CH:5]1[CH2:14][CH2:13][C:12]2[C:7](=[C:8]([NH2:17])[CH:9]=[C:10]([F:16])[C:11]=2[CH3:15])[C:6]1=[O:21])(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 61680MAGNESIUM SILICATE (synthetic)HCID 22080992N,N'-(3-Fluoro-4-methyl-8-oxo-5,6,7,8-tetrahydronaphthalene-1,7-diyl)diacetamide

生成物 1

HCID 10220585N-(8-Amino-6-fluoro-5-methyl-1-oxo-1,2,3,4-tetrahydronaphthalen-2-yl)acetamide収率 49.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

To 8.0 g of 2,8-diacetylamino-6-fluoro-5-methyl-1 -tetralone, 120 ml of a 20% aqueous solution of hydrochloric acid were added and the mixture was stirred at an external temperature of 60° C. for 2 hours. After the completion of the reaction, the reaction mixture was cooled and was added with 100 ml of water. The resulting mixture was filtered through a Kiriyama funnel. To the filtrate, further 100 ml of water were added, followed by extraction with chloroform. To the chloroform layer so obtained, potassium carbonate and Florisil were added and they were stirred for a while. The resulting mixture was filtered and then, the solvent was removed under reduced pressure. The residue so obtained was recrystallized from chloroform-diethyl ether, whereby 3.4 g of the title compound was obtained.

後処理

  1. customAfter the completion of the reaction
  2. temperaturethe reaction mixture was cooled
  3. filtrationThe resulting mixture was filtered through a Kiriyama funnel
  4. additionTo the filtrate, further 100 ml of water were added
  5. extractionfollowed by extraction with chloroform
  6. customTo the chloroform layer so obtained
  7. stirringthey were stirred for a while
  8. filtrationThe resulting mixture was filtered
  9. customthe solvent was removed under reduced pressure
  10. customThe residue so obtained
  11. customwas recrystallized from chloroform-diethyl ether

出典と根拠

ORDレコード
ord-98049c7fd27445eb97fca3f5795de2e8
出典データセット
uspto-grants-1998_12
特許番号
US05849945

反応ノート

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