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

HRID 58227

反応式

HRID 58227 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-a1eeb1a05eea429c80941a58897a5dc5
出典データセット
uspto-grants-2016_09
特許番号
US09434746B2

関連ノート

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