Pyrrolidine → 1-[2-(3-Methoxy-4-nitrophenyl)ethyl]pyrrolidine

HRID 871890노트

반응식

HRID 871890 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH:9]=[CH2:10])[CH:6]=[CH:5][C:4]=1[N+:11]([O-:13])=[O:12].[NH:14]1[CH2:18][CH2:17][CH2:16][CH2:15]1>CO>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH2:9][CH2:10][N:14]2[CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:6]=[CH:5][C:4]=1[N+:11]([O-:13])=[O:12]

참가 물질

4

반응물 2

HCID 31268PyrrolidineHCID 536287222-Methoxy-1-nitro-4-vinylbenzene

생성물 1

HCID 673259461-[2-(3-Methoxy-4-nitrophenyl)ethyl]pyrrolidine수율 75%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
100 °C

실험 절차

3.07 g (17.17 mmol) of the product prepared in step 24.1 and 7.13 mL (85.84 mL) of pyrrolidine in 60 mL of anhydrous methanol are placed in a sealed tube. The mixture is heated under pressure at 100°C. for 4 hours. After cooling to room temperature, it is evaporated to dryness. The residue obtained is purified by chromatography on a column of silica, eluting with a dichloromethane/methanol gradient (100/0 to 90/10). 3.22 g of the expected product are obtained in the form of a yellow solid. Yield=75%.

후처리

  1. temperatureAfter cooling to room temperature
  2. customit is evaporated to dryness
  3. customThe residue obtained
  4. customis purified by chromatography on a column of silica
  5. washeluting with a dichloromethane/methanol gradient (100/0 to 90/10)

출처 및 근거

ORD 기록
ord-b84e8ff85c2e4944b67dca9bd835a855
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975250B2

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