Dichloromethane → 2-(1-aminopropyl)-6-methyl-3-phenyl-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 58227

반응식

HRID 58227 반응식
[N:1]([CH:4]([C:7]1[N:8]=[C:9]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[N:10]2[C:11](=[O:19])[C:12]=1[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:5][CH3:6])=[N+]=[N-].CP(C)C.C(Cl)Cl>O1CCCC1.O>[NH2:1][CH:4]([C:7]1[N:8]=[C:9]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[N:10]2[C:11](=[O:19])[C:12]=1[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)[CH2:5][CH3:6]

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 68983TrimethylphosphineHCID 866500632-(1-azidopropyl)-6-methyl-3-phenyl-4H-pyrido[1,2-a]pyrimidin-4-one

생성물 1

HCID 668636882-(1-aminopropyl)-6-methyl-3-phenyl-4H-pyrido[1,2-a]pyrimidin-4-one

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

To a stirred solution of 2-(1-azidopropyl)-6-methyl-3-phenyl-4H-pyrido[1,2-a]pyrimidin-4-one (0.030 g, 0.094 mmol) in tetrahydrofuran (0.24 mL) and water (0.06 mL) was added 1.0 M of trimethylphosphine in tetrahydrofuran (0.11 mL) at room temperature and the mixture was stirred at room temperature for 1 hour. To the mixture was added methylene chloride and the mixture was washed with brine, dried over magnesium sulfate, and evaporated to dryness under reduced pressure. The crude residue was used directly in next step. LCMS calculated for C18H20N3O (M+H)+: m/z=294.2. Found: 294.3.

후처리

  1. washthe mixture was washed with brine
  2. dry with materialdried over magnesium sulfate
  3. customevaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-a1eeb1a05eea429c80941a58897a5dc5
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434746B2

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