Toluene → Benzphetamine Hydrochloride

HRID 2354147ノート

反応式

HRID 2354147 の反応式
[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]

参加物

6

反応物 4

HCID 1140Toluene2 回HCID 7503Benzyl ChlorideHCID 10340Sodium CarbonateHCID 10836Methamphetamine

生成物 1

HCID 11558159Benzphetamine Hydrochloride収率 69.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

To a 100 ml 3-neck flask was added 25.07 g (0.1680 mole) of methamphetamine, 24.26 g (0.2289 mole) of sodium carbonate and 13.58 g of toluene. The mixture was stirred and heated to 120° C. Then 23.04 g (0.1820 mole) of benzyl chloride was added over 53 minutes. The reaction was continued for a total of 12 hr. After the reaction was completed the mixture was cooled to ambient temperature and 75 g of toluene and 150 g of water were added. After aggressively mixing the layers were separated and the water layer was washed twice with 30 ml portions of toluene. To the combined toluene layers was added 12.04 g of concentrated hydrochloric acid affording a pH of 1 in the water layer. The entire mixture was transferred to a 500 ml 3-neck flask fitted with a mechanical stirrer, Dean-Stark trap and condenser. The water was removed by azeotropic distillation. The benzphetamine hydrochloride crystallized upon cooling 60° C. to about 40° C. Filtration afforded 28.34 g (0.1027 mole) of benzphetamine HCl which is a 61% yield. The benzphetamine HCl had a melting point of 150.3-152.4° C.

後処理

  1. customwas continued for a total of 12 hr
  2. temperaturewas cooled to ambient temperature
  3. additionAfter aggressively mixing the layers
  4. customwere separated
  5. washthe water layer was washed twice with 30 ml portions of toluene
  6. additionTo the combined toluene layers was added 12.04 g of concentrated hydrochloric acid affording a pH of 1 in the water layer
  7. customThe entire mixture was transferred to a 500 ml 3-neck flask
  8. customfitted with a mechanical stirrer
  9. customThe water was removed by azeotropic distillation
  10. customThe benzphetamine hydrochloride crystallized
  11. temperatureupon cooling 60° C. to about 40° C
  12. filtrationFiltration

出典と根拠

ORDレコード
ord-df82df5a37cf4ce08aaebaae7b3ea46e
出典データセット
uspto-grants-2010_07
特許番号
US07750187B2

反応ノート

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