HCID 18623221, 화합물 → 3-(3,4-Difluorophenyl)morpholine

HRID 278926노트

반응식

HRID 278926 반응식
[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]

참가 물질

5

반응물 2

HCID 18623221HCID 18623221, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 186232193-(3,4-Difluorophenyl)morpholine

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c6cdbf0a64174b12acb5666fe5d1551e
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06362182B1

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