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

HRID 355980ノート

反応式

HRID 355980 の反応式
[NH2:1][CH:2]1[CH2:11][CH2:10][C:9]2[C:4](=[C:5]([NH2:14])[CH:6]=[C:7]([F:13])[C:8]=2[CH3:12])[C:3]1=[O:15].C(O)C.C([O:21][C:22](=O)[C:23]([F:26])([F:25])[F:24])C.Cl>C(N(CC)CC)C.C1COCC1>[NH2:14][C:5]1[CH:6]=[C:7]([F:13])[C:8]([CH3:12])=[C:9]2[C:4]=1[C:3](=[O:15])[CH:2]([NH:1][C:22](=[O:21])[C:23]([F:26])([F:25])[F:24])[CH2:11][CH2:10]2

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 9794Ethyl trifluoroacetateHCID 22449502HCID 22449502、化合物

生成物 1

HCID 22449445N-(8-Amino-6-fluoro-5-methyl-1-oxo-1,2,3,4-tetrahydronaphthalen-2-yl)-2,2,2-trifluoroacetamide

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

反応条件

温度
20 °C

実験手順

The compound obtained in (8) above (1.66 gm) was dissolved into a mixed solvent of 70 ml of ethanol and 10 ml of THF. To the solution were added 2 ml of triethylamine and 1.5 ml of ethyltrifluoroacetate, followed by stirring for 20 hours at 20° C. The reaction product was added to dilute aqueous solution of hydrochloric acid and extracted with chloroform. The extract was washed with water, saturated sodium bicarbonate and saturated brine in this order, and dried over anhydrous sodium sulfate. After removal of the solvent by evaporation, the residue was subjected to silica gel column chromatography using chloroform as an eluant to obtain fractions containing the target compound. The fractions were concentrated to obtain 1.79 gm of the title compound.

後処理

  1. extractionextracted with chloroform
  2. washThe extract was washed with water, saturated sodium bicarbonate and saturated brine in this order
  3. dry with materialdried over anhydrous sodium sulfate
  4. customAfter removal of the solvent
  5. customby evaporation
  6. customto obtain fractions
  7. additioncontaining the target compound
  8. concentrationThe fractions were concentrated

出典と根拠

ORDレコード
ord-a3be8434b4f84c76907dbada209cd206
出典データセット
uspto-grants-1998_11
特許番号
US05834476

反応ノート

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