HCID 18623221、化合物 → 3-(3,4-Difluorophenyl)morpholine

HRID 278926ノート

反応式

HRID 278926 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[F:7][C:8]1[CH:9]=[C:10]([CH:15]2[NH:20][C:19](=O)[CH2:18][O:17][CH2:16]2)[CH:11]=[CH:12][C:13]=1[F:14]>CCOCC.C1COCC1>[F:7][C:8]1[CH:9]=[C:10]([CH:15]2[NH:20][CH2:19][CH2:18][O:17][CH2:16]2)[CH:11]=[CH:12][C:13]=1[F:14]

参加物

5

反応物 2

HCID 18623221HCID 18623221、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 186232193-(3,4-Difluorophenyl)morpholine

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

To a suspension of LiAlH4 (6.0 mmol, 0.23 g) in 25.0 mL of Et2O was added a solution of 5-(3,4-difluoro-phenyl)-morpholin-3-one (2.0 mmol, 0.42 g) in 20.0 mL Et2O and 5.0 mL THF at room temperature. The resulting suspension was heated to reflux for 2 hours and was then quenched with water and aq. NaOH solution. The solid was filtered off and the filtrate was dried over Na2SO4. The filtrate was then decanted and the solvent was removed in vacuo to obtain 5-(3,4-difluoro-phenyl)-morpholine as a viscous oil. It was converted to its hydrochloride salt for its analysis. Yellow powder. M.P.=171-173° C.; Mass spec. 200 (M+1, 100%). Analysis calculated for C10H12NOF2Cl.0.5 acetone: C, 51.96; H, 5.61; N, 5.41. Found: C, 51.98; H, 5.70; N, 5.34.

後処理

  1. temperatureThe resulting suspension was heated
  2. temperatureto reflux for 2 hours
  3. customwas then quenched with water and aq. NaOH solution
  4. filtrationThe solid was filtered off
  5. dry with materialthe filtrate was dried over Na2SO4
  6. customThe filtrate was then decanted
  7. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-c6cdbf0a64174b12acb5666fe5d1551e
出典データセット
uspto-grants-2002_03
特許番号
US06362182B1

反応ノート

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