Morpholine → 4-(2-Bromo-4-fluorobenzyl)morpholine

HRID 558140노트

반응식

HRID 558140 반응식
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH2:9]Br.[NH:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1.C(N(C(C)C)CC)(C)C>C(#N)C>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[CH2:9][N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 81531DiisopropylethylamineHCID 107069772-Bromo-1-(bromomethyl)-4-fluorobenzene

생성물 1

HCID 510751744-(2-Bromo-4-fluorobenzyl)morpholine수율 95.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
81 °C

실험 절차

Combine 2-bromo-1-bromomethyl-4-fluoro-benzene (4 g, 14.9 mmol), morpholine (2.6 mL, 29.8 mmol), and diisopropylethylamine (5.2 mL, 29.8 mmol) in acetonitrile (10.0 mL). Heat the reaction mixture at 81° C. for 2 h and cool to RT. Remove the solvent under reduced pressure. Dilute with DCM and wash with water and then aqueous saturated sodium chloride. Dry the organics over sodium sulfate. Filter and remove the solvent under reduced pressure to obtain the title compound (3.9 g, 95%). LCMS (ES) m/z 274 [M+1]+.

후처리

  1. temperaturecool to RT
  2. customRemove the solvent under reduced pressure
  3. additionDilute with DCM
  4. washwash with water
  5. dry with materialDry the organics over sodium sulfate
  6. filtrationFilter
  7. customremove the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-d0b7435402014f4f8423aa7233a3c960
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063035B2

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