Tetrahydrofuran → 4-(3-Bromo-5-nitropyridin-2-yl)morpholine

HRID 340459노트

반응식

HRID 340459 반응식
C(N(CC)CC)C.[NH:8]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1.O1CCCC1.[Br:19][C:20]1[C:21](Cl)=[N:22][CH:23]=[C:24]([N+:26]([O-:28])=[O:27])[CH:25]=1>O>[Br:19][C:20]1[C:21]([N:8]2[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[N:22][CH:23]=[C:24]([N+:26]([O-:28])=[O:27])[CH:25]=1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 8083MorpholineHCID 8471TriethylamineHCID 2308893-Bromo-2-chloro-5-nitropyridine

생성물 1

HCID 467388804-(3-Bromo-5-nitropyridin-2-yl)morpholine수율 95.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Triethylamine (191 mg) and morpholine (120 mg) were added to a tetrahydrofuran (4 ml) solution containing 3-bromo-2-chloro-5-nitropyridine (300 mg), followed by stirring for 40 minutes. Water was added to the reaction solution, followed by extraction with ethyl acetate. The resultant was washed with saturated saline and dried over anhydrous sodium sulfate. Subsequently, the solvent was distilled away under reduced pressure, the obtained residue was purified by silica gel chromatography (chloroform:methanol=1:0 to 3:1), and a yellow solid of 4-(3-bromo-5-nitropyridin-2-yl)morpholine (346 mg) was thus obtained.

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe resultant was washed with saturated saline
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationSubsequently, the solvent was distilled away under reduced pressure
  5. customthe obtained residue was purified by silica gel chromatography (chloroform:methanol=1:0 to 3:1)

출처 및 근거

ORD 기록
ord-eb8b7dfd8b0d48b79b114a3dfd46462a
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895585B2

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