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

HRID 2421357노트

반응식

HRID 2421357 반응식
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6]Br)=[C:4]([F:10])[CH:3]=1.[NH:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1>CN(C)C=O>[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)=[C:4]([F:10])[CH:3]=1

참가 물질

4

반응물 2

HCID 8083MorpholineHCID 27336604-Bromo-2-fluorobenzyl bromide

생성물 1

HCID 219145034-(4-Bromo-2-fluorobenzyl)morpholine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-Bromo-2-fluorobenzyl bromide (3.0 g) and morpholine (2.15 ml) were stirred in dimethylformamide (30 ml) at ambient temperature for 18 h. The mixture was partitioned between diethyl ether (80 ml) and water (80 ml). The aqueous phase was extracted further with diethyl ether (80 ml) and the combined organic phases were dried (magnesium sulfate) and concentrated in vacuo. The residue was purified by column chromatography, eluting with a gradient of 0-30% ethyl acetate/iso-hexane to give the product as a colourless oil (2.92 g).

후처리

  1. customThe mixture was partitioned between diethyl ether (80 ml) and water (80 ml)
  2. extractionThe aqueous phase was extracted further with diethyl ether (80 ml)
  3. dry with materialthe combined organic phases were dried (magnesium sulfate)
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography
  6. washeluting with a gradient of 0-30% ethyl acetate/iso-hexane

출처 및 근거

ORD 기록
ord-fc119b72487d40b4896374ba98a3b5fb
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07956084B2

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