Hydrochloric Acid → (1S,2R)-(+)-Norephedrine

HRID 2188314ノート

反応式

HRID 2188314 の反応式
Cl.[C:2]1([CH:8]([OH:19])[CH:9]([NH:11]C(OC(C)(C)C)=O)[CH3:10])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CO>[C:2]1([CH:8]([OH:19])[CH:9]([NH2:11])[CH3:10])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

実験手順

20 ml of 3N-hydrochloric acid solution and 10 ml of methanol were added into the above-described 1-phenyl-2-(t-butoxycarbonylamino)propanol in an amount of 1.05 g (4.00 mmol), and the resulting solution was stirred for an hour at an ambient temperature. Then, the methanol in the solution was distilled out, and the aqueous layer of the solution was separated by extraction with ethyl acetate. The aqueous layer was adjusted to alkaline state by adding aqueous solution of sodium hydroxide and was then extracted with chloroform. The obtained chloroform solution was dried with anhydrous magnesium sulfate and distilled under reduced pressure to obtain 1-phenyl-2-aminopropanol in an amount of 465 mg (2.48 mmol) at a yield of 77%.

後処理

  1. distillationThen, the methanol in the solution was distilled out
  2. customthe aqueous layer of the solution was separated by extraction with ethyl acetate
  3. additionby adding aqueous solution of sodium hydroxide
  4. extractionwas then extracted with chloroform
  5. dry with materialThe obtained chloroform solution was dried with anhydrous magnesium sulfate
  6. distillationdistilled under reduced pressure

出典と根拠

ORDレコード
ord-bf59b5dc2a934e1f94c747864bb8ac70
出典データセット
uspto-grants-2002_06
特許番号
US06410749B1

反応ノート

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