HCID 57849580、化合物 → (2S)-2-Phenylmorpholine

HRID 2076800ノート

反応式

HRID 2076800 の反応式
C(OC([N:8]1[CH2:13][CH2:12][O:11][C@@H:10]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:9]1)=O)(C)(C)C>Cl.O1CCOCC1>[C:14]1([C@@H:10]2[O:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

4

反応物 1

HCID 57849580HCID 57849580、化合物

生成物 1

HCID 937783(2S)-2-Phenylmorpholine収率 77.8%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

1.280 g (S)-2-Phenyl-morpholine-4-carboxylic acid tert-butyl ester was dissolved in 31 mL 4N HCl in dioxane and stirred at room temperature overnight. Concentrated in vacuo and diluted with 1N HCl. The aqueous was extracted with ether and then basicified to pH 12-14 with 2N NaOH followed by extraction with DCM. The organic layers were dried over Na2SO4, filtered and concentrated in vacuo to afford 617 mg of product by H NMR. 78% yield.

後処理

  1. concentrationConcentrated in vacuo
  2. additiondiluted with 1N HCl
  3. extractionThe aqueous was extracted with ether
  4. extractionfollowed by extraction with DCM
  5. dry with materialThe organic layers were dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-bb26e92263f941a8ac5abc575829733c
出典データセット
uspto-grants-2011_04
特許番号
US07928103B2

反応ノート

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