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Water → 5-Fluoro-8-nitro-3,4-dihydronaphthalen-1(2H)-one

HRID 964656
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HRID 964656 반응식
[F:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][C:7]2=[O:12].[N+:13]([O-])([O-:15])=[O:14].[K+].O>S(=O)(=O)(O)O>[F:1][C:2]1[CH:11]=[CH:10][C:9]([N+:13]([O-:15])=[O:14])=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][C:7]2=[O:12]
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참가 물질

5

반응물 3

HCID 962WaterHCID 24434Potassium NitrateHCID 154910385-Fluoro-1,2,3,4-tetrahydronaphthalen-1-one

생성물 1

HCID 224494055-Fluoro-8-nitro-3,4-dihydronaphthalen-1(2H)-one

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

14 gm of the compound prepared in (7) above was dissolved into 100 ml of concentrated sulfuric acid. After cooling the solution, a solution of 9.05 gm of potassium nitrate in 80 ml of concentrated sulfuric acid was added dropwise while maintaining the internal temperature below 5° C. The stirring was continued for a further 30 minutes. The resultant reaction mixture was poured into ice-cooled water and extracted with chloroform. The extract was washed with saturated aqueous solution of sodium bicarbonate, water, and saturated brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated and residue was recrystallized in methanol to obtain 9.15 gm of the title compound.

후처리

  1. temperatureAfter cooling the solution
  2. temperaturewhile maintaining the internal temperature below 5° C
  3. customThe resultant reaction mixture
  4. additionwas poured into ice-
  5. extractionextracted with chloroform
  6. washThe extract was washed with saturated aqueous solution of sodium bicarbonate, water, and saturated brine in this order
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe solvent was evaporated
  9. customresidue was recrystallized in methanol

출처 및 근거

ORD 기록
ord-853c0253bc8a49759d27b6cb2a489cd2
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05770605

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