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Triethylamine → HCID 22147131, 화합물

HRID 1824446
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HRID 1824446 반응식
C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)C=CC=CC=1.C(N(CC)CC)C.[C:25]([C:29]1[CH:30]=[C:31](C(O)=O)[N:32]([C:34]2[CH:35]=[N:36][C:37]([CH3:40])=[N:38][CH:39]=2)[N:33]=1)([CH3:28])([CH3:27])[CH3:26].C(C1C=C([NH:54][C:55]([NH:57][C:58]2[C:67]3[C:62](=[CH:63][CH:64]=[CH:65][CH:66]=3)[C:61]([O:68][C:69]3[CH:74]=[CH:73][N:72]=[C:71]([NH:75][CH2:76][CH:77]4[CH2:79][CH2:78]4)[N:70]=3)=[CH:60][CH:59]=2)=[O:56])N(C)N=1)(C)(C)C>C(COC)OC.C1COCC1>[C:25]([C:29]1[CH:30]=[C:31]([NH:54][C:55]([NH:57][C:58]2[C:67]3[C:62](=[CH:63][CH:64]=[CH:65][CH:66]=3)[C:61]([O:68][C:69]3[CH:74]=[CH:73][N:72]=[C:71]([NH:75][CH2:76][CH:77]4[CH2:79][CH2:78]4)[N:70]=3)=[CH:60][CH:59]=2)=[O:56])[N:32]([C:34]2[CH:39]=[N:38][C:37]([CH3:40])=[N:36][CH:35]=2)[N:33]=1)([CH3:26])([CH3:27])[CH3:28]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 22147130HCID 22147130, 화합물HCID 22147192HCID 22147192, 화합물

생성물 1

HCID 22147131HCID 22147131, 화합물수율 7%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran
용매
HCID 80711,2-Dimethoxyethane용매

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온도
85 °C

실험 절차

Diphenylphosphoryl azide (DPPA) (0.09 mL, 0.423 mmol, 1.1 equiv.) and triethylamine (0.075 mL, 0.54 mmol, 1.4 equiv.) were added to 5-tert-butyl-2-(2-methylpyrimidin-5-yl)-2H-pyrazole-3-carboxylic acid (100 mg, 0.384 mmol, 1.0 equiv.) in 2.0 mL anhydrous dimethoxyethane in a sealed tube. The mixture was heated at 85° C. for 2.5 h, then a solution of the cyclopropylmethylaminopyrimidine-ether intermediate (see Example 4)(118 mg, 0.38 mmol, 1.0 equiv.) in 3.0 mL anhydrous THF was added and the resulting mixture stirred at room temperature overnight. The solvent was removed in vacuo and the crude urea was purified by column chromatography on silica gel using 0–65% EtOAc in hexanes eluent mixtures. The product was purified further by prep-HPLC affording 15 mg of the title compound (7% yield).

후처리

  1. customThe solvent was removed in vacuo
  2. customthe crude urea was purified by column chromatography on silica gel using 0–65% EtOAc in hexanes eluent mixtures
  3. customThe product was purified further

출처 및 근거

ORD 기록
ord-a2b66615ab3e40e0aac226bbf03d4dd8
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07041669B2

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