Triethylamine → 4-Chloro-2,6-dimethyl-5-{[4-(trifluoromethyl)phenyl]ethynyl}pyrimidine

HRID 339745

반응식

HRID 339745 반응식
[CH3:1][C:2]1[NH:7][C:6](=O)[C:5](I)=[C:4]([CH3:10])[N:3]=1.[C:11]([C:13]1[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][CH:14]=1)#[CH:12].C(N(CC)CC)C.O=P(Cl)(Cl)[Cl:32]>C1(C)C=CC=CC=1.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[Cl:32][C:6]1[C:5]([C:12]#[C:11][C:13]2[CH:18]=[CH:17][C:16]([C:19]([F:20])([F:21])[F:22])=[CH:15][CH:14]=2)=[C:4]([CH3:10])[N:3]=[C:2]([CH3:1])[N:7]=1

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 43482951-Ethynyl-4-(trifluoromethyl)benzeneHCID 1354479355-Iodo-2,6-dimethylpyrimidin-4-ol

생성물 1

HCID 866607064-Chloro-2,6-dimethyl-5-{[4-(trifluoromethyl)phenyl]ethynyl}pyrimidine

시약·촉매·용매 2

HCID 178418476HCID 178418476, 화합물촉매HCID 1140Toluene용매

실험 절차

2,6-Dimethyl-5-iodo-4(3H)-pyrimidinone and 4-ethynyl-α,α,α-trifluorotoluene were reacted in toluene in the presence of dichlorobis(triphenylphosphine)palladium, cuprous iodide, and triethylamine while stirring under room temperature to heating to obtain a compound. The compound was mixed with POCl3 and reacted while heating under reflux to obtain a target substance. The target substance was subjected to e.g., proton nuclear magnetic resonance spectrometry (1H-NMR) and mass spectrometry (MS) and confirmed as the titled compound. Furthermore, MS measurement result is shown.

후처리

  1. temperatureto heating
  2. customto obtain a compound
  3. customreacted
  4. temperaturewhile heating
  5. temperatureunder reflux
  6. customto obtain a target substance

출처 및 근거

ORD 기록
ord-821eedf0fb894a2ba9087b8285f1b445
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895565B2

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