Triethylamine → 4-Chloro-2-cyclopropyl-5-nitropyrimidine

HRID 2175200ノート

反応式

HRID 2175200 の反応式
[CH:1]1([C:4]2[NH:9][C:8](=O)[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][N:5]=2)[CH2:3][CH2:2]1.C(N(CC)CC)C.P(Cl)(Cl)([Cl:23])=O>ClCCl>[Cl:23][C:8]1[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][N:5]=[C:4]([CH:1]2[CH2:3][CH2:2]2)[N:9]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 584974342-cyclopropyl-5-nitro-3H-pyrimidin-4-one

生成物 1

HCID 567734194-Chloro-2-cyclopropyl-5-nitropyrimidine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of the 2-cyclopropyl-5-nitro-3H-pyrimidin-4-one (900 mg, 4.9 mmol) in dichloromethane (15 ml) was added triethylamine (505 mg, 5 mmol). To the clear solution obtained, phosphorous oxychloride (1.5 g, 10 mmol) was slowly added and the reaction mixture kept at room temperature for 2 hours. TLC showed a single spot. The reaction mixture was diluted with dichloromethane, washed with water and dried over MgSO4, filtered and evaporated to dryness to give brown oil. This material was used as such for the next step.

後処理

  1. customTo the clear solution obtained
  2. washwashed with water
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customto give brown oil

出典と根拠

ORDレコード
ord-834e20c56f5f441aa57c6800731ed1ed
出典データセット
uspto-grants-2015_06
特許番号
US09062056B2

反応ノート

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