Sodium Hydroxide → 4-[(1,3-Difluoropropan-2-yl)oxy]aniline

HRID 1655547ノート

反応式

HRID 1655547 の反応式
[F:1][CH2:2][CH:3]([O:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-])=O)=[CH:9][CH:8]=1)[CH2:4][F:5].Cl[Sn]Cl.[OH-].[Na+]>C(O)C>[F:1][CH2:2][CH:3]([O:6][C:7]1[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=1)[CH2:4][F:5]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24479Stannous ChlorideHCID 54192518HCID 54192518、化合物

生成物 1

HCID 534245344-[(1,3-Difluoropropan-2-yl)oxy]aniline

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3.4 g (15.7 mmol) of p-(1,3-difluoro-2-propoxy)nitrobenzene, 17.7 g (78.5 mmol) of SnCl2 ·2H2O and 35 ml of absolute ethanol were heated together at reflux for 1 hour. The reaction mixture was poured over ice, made basic with 50 percent aqueous NaOH and extracted three times into ether. The combined ether extracts were washed two times with water, dried over MgSO4 and filtered. Hydrogen chloride gas was bubbled into the ether solution causing the above-named aniline to precipitate as the hydrochloride salt. The product was collected as a tan solid by filtration (80 percent of theoretical) and decomposed (d) at 240° C. T1 - % C? % H? % N? -Analysis: -Calc. for C9H11F2NO.HCl: 48.33 5.41 6.26 -Found: 48.42 5.41 6.33 -

後処理

  1. temperatureat reflux for 1 hour
  2. additionThe reaction mixture was poured over ice
  3. extractionextracted three times into ether
  4. washThe combined ether extracts were washed two times with water
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customHydrogen chloride gas was bubbled into the ether solution
  8. customto precipitate as the hydrochloride salt
  9. filtrationThe product was collected as a tan solid by filtration (80 percent of theoretical)
  10. customat 240° C

出典と根拠

ORDレコード
ord-9acd510732364543bec6f0b75bb73a0f
出典データセット
uspto-grants-1993_10
特許番号
US05250690

反応ノート

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