Toluene → Benzphetamine Hydrochloride

HRID 2354146

반응식

HRID 2354146 반응식
[CH3:1][C@H:2]([NH:10][CH3:11])[CH2:3][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.C(=O)([O-])[O-].[Na+].[Na+].[C:18]1([CH3:24])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C([Cl:32])C1C=CC=CC=1>O>[CH3:1][C@H:2]([N:10]([CH2:24][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[CH3:11])[CH2:3][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.[ClH:32]

참가 물질

6

반응물 4

HCID 1140Toluene2회HCID 7503Benzyl ChlorideHCID 10340Sodium CarbonateHCID 10836Methamphetamine

생성물 1

HCID 11558159Benzphetamine Hydrochloride수율 70%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
120 °C

실험 절차

To a 100 ml 3-neck flask fitted with a mechanical stirrer was added 17.10 g (0.1145 moles) of methamphetamine, 14.50 g (0.1368 mole) of sodium carbonate and 10.60 g of toluene. The reaction mass was heated to 120° C. and 16.18 g (0.1265 mole) of benzyl chloride was added over 180 minutes. The reaction was continued for a total of 6.75 hr. The reaction mass was cooled and transferred to a 500 ml flask equipped with a mechanical stirrer. To this flask was added 45 ml of toluene and 90 ml of water. The mixture was aggressively stirred to dissolve the salt. The layers were separated and the water layer was washed twice with 20 ml portions of toluene. The combined toluene layers were washed with 20 ml of water. Then to the stirred toluene layer was added 11.33 g of concentrated hydrochloric acid. The flask was equipped with a Dean-Stark trap and condenser and the water was removed by azeotropic distillation. There was 8.9 g of water recovered from the Dean-Stark trap. The organic material crystallized upon cooling between about 60° C. to about 40° C. affording 19.79 g of crude benzphetamine hydrochloride which is a 70% yield.

후처리

  1. customTo a 100 ml 3-neck flask fitted with a mechanical stirrer
  2. customwas continued for a total of 6.75 hr
  3. temperatureThe reaction mass was cooled
  4. customtransferred to a 500 ml flask
  5. customequipped with a mechanical stirrer
  6. dissolutionto dissolve the salt
  7. customThe layers were separated
  8. washthe water layer was washed twice with 20 ml portions of toluene
  9. washThe combined toluene layers were washed with 20 ml of water
  10. additionThen to the stirred toluene layer was added 11.33 g of concentrated hydrochloric acid
  11. customThe flask was equipped with a Dean-Stark trap and condenser
  12. customthe water was removed by azeotropic distillation
  13. customrecovered from the Dean-Stark trap
  14. customThe organic material crystallized
  15. temperatureupon cooling between about 60° C. to about 40° C.

출처 및 근거

ORD 기록
ord-7202b0351b26437db630c823e82a8943
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07750187B2

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