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

HRID 2175200노트

반응식

HRID 2175200 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-834e20c56f5f441aa57c6800731ed1ed
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09062056B2

반응 노트

불러오는 중…