2-Methoxyethylamine → HCID 22335356, 화합물

HRID 586713노트

반응식

HRID 586713 반응식
[CH2:1]([N:8]1[CH2:17][CH2:16][C:15]2[N:14]=[C:13](Cl)[CH:12]=[CH:11][C:10]=2[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:19][O:20][CH2:21][CH2:22][NH2:23]>S([O-])([O-])(=O)=O.[Cu+2]>[CH2:1]([N:8]1[CH2:17][CH2:16][C:15]2[N:14]=[C:13]([NH:23][CH2:22][CH2:21][O:20][CH3:19])[CH:12]=[CH:11][C:10]=2[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 80182-MethoxyethylamineHCID 162287476-Benzyl-2-chloro-5,6,7,8-tetrahydro-1,6-naphthyridine

생성물 1

HCID 22335356HCID 22335356, 화합물

시약·촉매·용매 1

HCID 24462Copper Sulfate촉매

실험 절차

Copper (II) sulphate (200 mg) was added to a solution of 6-benzyl-2-chloro-5,6,7,8-tetrahydro-[1,6]naphthyridine (4.5 g, 17.4 mmol)(see reference WO9830560 Example 33 b) in 2-methoxyethylamine and the mixture was heated under reflux for 20 hours. The mixture was evaporated under reduced pressure and the residue was partitioned between dichloromethane (100 ml) and water (50 ml). The aqueous phase was extracted with dichloromethane (2×50 ml) and the combined organic phases were dried over magnesium sulphate and evaporated under reduced pressure. The residue was purified by chromatography on silica gel using methanol in dichloromethane as eluant (gradient from 1:99 to 3:97) to give the title compound as an orange oil (1.32 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 20 hours
  3. customThe mixture was evaporated under reduced pressure
  4. customthe residue was partitioned between dichloromethane (100 ml) and water (50 ml)
  5. extractionThe aqueous phase was extracted with dichloromethane (2×50 ml)
  6. dry with materialthe combined organic phases were dried over magnesium sulphate
  7. customevaporated under reduced pressure
  8. customThe residue was purified by chromatography on silica gel

출처 및 근거

ORD 기록
ord-1cc2ad42002b44ce974a6abef9d1d76f
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936619B2

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