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Phenylethanolamine → HCID 13713311、化合物

HRID 231852
ノート
印刷プレビュー

反応式

HRID 231852 の反応式
NCC(C1C=CC=CC=1)O.[N+](C1C=CC(CCC(C)=O)=CC=1)([O-])=O.C1(C)C=CC(S(O)(=O)=O)=CC=1.Cl.[C:37]1([CH:43]([OH:59])[CH2:44][NH:45][CH:46]([CH3:58])[CH2:47][CH2:48][C:49]2[CH:54]=[CH:53][C:52]([N+:55]([O-:57])=[O:56])=[CH:51][CH:50]=2)[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1>O.C1(C)C=CC=CC=1>[C:37]1([CH:43]([OH:59])[CH2:44][NH:45][CH:46]([CH3:58])[CH2:47][CH2:48][C:49]2[CH:50]=[CH:51][C:52]([N+:55]([O-:57])=[O:56])=[CH:53][CH:54]=2)[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1000PhenylethanolamineHCID 6101p-Toluenesulfonic acidHCID 122356724-(4-Nitrophenyl)butan-2-oneHCID 13713312HCID 13713312、化合物

生成物 1

HCID 13713311HCID 13713311、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 1140
Toluene
溶媒

実験手順

A solution of 5.0 g. (25.9 mM) of 2-amino-1-phenylethanol and 3.55 g. (25.9 mM) of methyl 2-(4-nitrophenyl)ethyl ketone in 60 ml. of toluene containing 10 mg. of para-toluenesulfonic acid was heated at reflux for six hours in a flask equipped with a Dean-Stark trap. The water that formed during the reaction was removed via the trap, and then the reaction mixture was cooled to room temperature and concentrated to dryness by evaporation of the solvent under reduced pressure. The solid product that remained was dissolved in 50 ml. of tetrahydrofuran and the solution was heated to reflux. A solution of 13.5 ml. of 2N borane-methyl sulfide complex in tetrahydrofuran was then added dropwise to the reaction mixture, and the mixture was refluxed for an additional ninety minutes. After cooling the reaction mixture to room temperature, it was diluted by addition of diethyl ether saturated with hydrogen chloride. The precipitate that was formed was collected by filtration and crystallized from ethanol and diethyl ether to give 3.29 g. of 1-phenyl- 2-[1-methyl-3-(4-nitrophenyl)-propylamino]ethanol hydrochloride. M.P. 203°-213° C.

後処理

  1. temperatureat reflux for six hours in a flask
  2. customequipped with a Dean-Stark trap
  3. customwas removed via the trap
  4. concentrationconcentrated to dryness by evaporation of the solvent under reduced pressure
  5. dissolutionThe solid product that remained was dissolved in 50 ml
  6. temperatureof tetrahydrofuran and the solution was heated to reflux
  7. additionof 2N borane-methyl sulfide complex in tetrahydrofuran was then added dropwise to the reaction mixture
  8. temperaturethe mixture was refluxed for an additional ninety minutes
  9. temperatureAfter cooling the reaction mixture to room temperature
  10. additionit was diluted by addition of diethyl ether saturated with hydrogen chloride
  11. customThe precipitate that was formed
  12. filtrationwas collected by filtration
  13. customcrystallized from ethanol and diethyl ether
  14. customto give 3.29 g

出典と根拠

ORDレコード
ord-1668623e290248fb93dabcd2920a72f2
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04849453

反応ノート

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