Triethylamine → Ethyl 5-(6-methyl-5-{[4-(trifluoromethyl)phenyl]ethynyl}pyrimidin-4-ylaminomethyl)-2-furancarboxylate

HRID 339748노트

반응식

HRID 339748 반응식
[NH2:1][C:2]1[C:7]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]([F:19])([F:18])[F:17])=[CH:12][CH:11]=2)=[C:6]([CH3:20])[N:5]=[CH:4][N:3]=1.C(N(CC)CC)C.Cl[CH2:29][C:30]1[O:34][C:33]([C:35]([O:37][CH2:38][CH3:39])=[O:36])=[CH:32][CH:31]=1>C1(C)C=CC=CC=1>[CH3:20][C:6]1[N:5]=[CH:4][N:3]=[C:2]([NH:1][CH2:29][C:30]2[O:34][C:33]([C:35]([O:37][CH2:38][CH3:39])=[O:36])=[CH:32][CH:31]=2)[C:7]=1[C:8]#[C:9][C:10]1[CH:11]=[CH:12][C:13]([C:16]([F:19])([F:17])[F:18])=[CH:14][CH:15]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 263166Ethyl 5-(chloromethyl)-2-furancarboxylateHCID 680024494-Amino-6-methyl-5-{[4-(trifluoromethyl)phenyl]ethynyl}pyrimidine

생성물 1

HCID 44815753Ethyl 5-(6-methyl-5-{[4-(trifluoromethyl)phenyl]ethynyl}pyrimidin-4-ylaminomethyl)-2-furancarboxylate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 4-amino-6-methyl-5-{[4-(trifluoromethyl)phenyl]ethynyl}pyrimidine (2 g), triethylamine (0.76 g), ethyl 5-chloromethyl-2-furancarboxylate (1.4 g) and toluene (60 ml) was heated to reflux while stirring for 10 hours. The mixture thus obtained was concentrated under reduced pressure. After the resultant residue was washed with water added thereto, an organic phase was dried over anhydrous sodium sulfate and evaporated. The resultant residue was purified by column chromatography to obtain a target substance (0.6 g). 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. temperaturewas heated
  2. temperatureto reflux
  3. customThe mixture thus obtained
  4. concentrationwas concentrated under reduced pressure
  5. washAfter the resultant residue was washed with water
  6. additionadded
  7. dry with materialan organic phase was dried over anhydrous sodium sulfate
  8. customevaporated
  9. customThe resultant residue was purified by column chromatography
  10. customto obtain a target substance (0.6 g)

출처 및 근거

ORD 기록
ord-66bc838d098f43808e93105c7ec6a987
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895565B2

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