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

HRID 2186883노트

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HRID 2186883 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 9794Ethyl trifluoroacetateHCID 22449502HCID 22449502, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

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온도
20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9d2dc2f452ea40bd9732c4521f832e20
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06407115B1

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