Water → Methamphetamine

HRID 58515

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HRID 58515 반응식
[NH2:1][CH:2]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH3:3].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[CH:18](OCC)=O>C(OCC)C>[CH3:3][C@H:2]([NH:1][CH3:18])[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

참가 물질

6

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온도
100 °C

실험 절차

Amphetamine free base (100 mg, 0.71 mmol) was dissolved in ethyl formate (10 mL). The solution was heated under pressure in an ACE pressure reactor for 2 hours at 100° C. The reaction mixture was cooled down, and the solvent was evaporated under reduced pressure. The resulting carbamate derivative was dissolved in dried diethyl ether (5 mL). The solution was added dropwise to a suspension of lithium aluminium hydride (40.4 mg, 1.07 mmol) in diethyl ether (10 mL). The reaction mixture was refluxed for 5 hours. Thereafter, water was carefully added after the reaction mixture had been cooled down to 0° C. on an ice bath. The lithium salt was filtered over Celite™ diatomaceous earth in Buchner funnel. The granules obtained were washed thoroughly with excess diethyl ether. The combined ether phases were washed with 5% sodium hydroxide and brine before being dried with magnesium sulfate. The solvent was evaporated to yield 96 mg methamphetamine free base.

후처리

  1. temperatureThe reaction mixture was cooled down
  2. customthe solvent was evaporated under reduced pressure
  3. dissolutionThe resulting carbamate derivative was dissolved in dried diethyl ether (5 mL)
  4. temperatureThe reaction mixture was refluxed for 5 hours
  5. temperaturehad been cooled down to 0° C. on an ice bath
  6. filtrationThe lithium salt was filtered over Celite™ diatomaceous earth in Buchner funnel
  7. customThe granules obtained
  8. washwere washed thoroughly with excess diethyl ether
  9. washThe combined ether phases were washed with 5% sodium hydroxide and brine
  10. dry with materialbefore being dried with magnesium sulfate
  11. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-508e7efaec174210812995a8dc33d617
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09435816B2

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