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Triethylamine → HCID 178511622, 화합물

HRID 1943476
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HRID 1943476 반응식
Cl[C:2]1[CH:3]=[C:4]([N:14](CC2C=CC(OC)=CC=2)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:5]2[N:6]([C:8]([C:11]([OH:13])=O)=[CH:9][N:10]=2)[N:7]=1.[F:30][C:31]1[CH:37]=[CH:36][C:34]([NH2:35])=[CH:33][CH:32]=1.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.C(N(CC)CC)C.[NH2:66][C@H:67]1[CH2:72][CH2:71][C@H:70]([NH2:73])[CH2:69][CH2:68]1>C(Cl)Cl.O.C(#N)C>[NH2:66][C@H:67]1[CH2:72][CH2:71][C@H:70]([NH:73][C:2]2[CH:3]=[C:4]([NH:14][C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:5]3[N:6]([C:8]([C:11]([NH:35][C:34]4[CH:36]=[CH:37][C:31]([F:30])=[CH:32][CH:33]=4)=[O:13])=[CH:9][N:10]=3)[N:7]=2)[CH2:69][CH2:68]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 8471TriethylamineHCID 97314-FluoroanilineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 596248836-Chloro-8-((4-methoxybenzyl)(phenyl)amino)imidazo[1,2-b]pyridazine-3-carboxylic acidHCID 178511674HCID 178511674, 화합물

생성물 1

HCID 178511622
HCID 178511622, 화합물
수율 32.6%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 21908982Water methylene chloride용매

실험 절차

In a 2 dram reaction vial containing acetonitrile (1 mL) at ambient temperature was added 6-chloro-8-((4-methoxybenzyl)(phenyl)amino)imidazo[1,2-b]pyridazine-3-carboxylic acid (0.025 g, 0.06 mmol), 4-fluoroaniline (0.010 g, 0.09 mmol), EDCI (0.018 g, 0.09 mmol), HOBt (0.012 g, 0.09 mmol), and triethylamine (0.025 mL, 0.18 mmol). The suspension was stirred overnight at room temperature. The reaction mixture was then concentrated in vacuo and the residue mixed with trans-1,4-diaminocyclohexane (0.5 g, 4.39 mmol) and heated to 160° C. for 5 h. After cooling to room temperature, the reaction mixture was diluted with DCM/water and the layers were separated. The organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was dissolved in DCM (1 mL) at room temperature and charged with TFA (1 mL). The mixture was stirred 3 h, whereupon the volatiles were removed via a stream of nitrogen and the crude mixture was purified via preparative HPLC (Waters Sunfire column 5u, 100 A°, 19×100 mm, 20-100% Solvent B, (Solvent A (90% water, 10% methanol, 0.1% TFA), Solvent B (10% water, 90% methanol, 0.1% TFA), 10 min gradient, 10 minute run, 25 mL/min)), affording the title compound, 6-((trans)-4-aminocyclohexylamino)-N-(4-fluorophenyl)-8-(phenylamino)imidazo[1,2-b]pyridazine-3-carboxamide (0.009 g, 22%). HPLC: Rt=3.04 min. (Waters sunfire 4.6×50 mm C18.5 um 4 min/1 min hold time 0-100% (A-B) A=10% MeOH-90% water-0.1% TFA, B=90% MeOH-10% water-0.1% TFA). MS: [M+H]=460.0.

후처리

  1. customIn a 2 dram reaction
  2. concentrationThe reaction mixture was then concentrated in vacuo
  3. temperatureheated to 160° C. for 5 h
  4. temperatureAfter cooling to room temperature
  5. customthe layers were separated
  6. dry with materialThe organic phase was dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. dissolutionThe residue was dissolved in DCM (1 mL) at room temperature
  10. additioncharged with TFA (1 mL)
  11. stirringThe mixture was stirred 3 h, whereupon the volatiles
  12. customwere removed via a stream of nitrogen
  13. customthe crude mixture was purified via preparative HPLC (Waters Sunfire column 5u, 100 A°, 19×100 mm, 20-100% Solvent B, (Solvent A (90% water, 10% methanol, 0.1% TFA), Solvent B (10% water, 90% methanol, 0.1% TFA), 10 min gradient, 10 minute run, 25 mL/min))

출처 및 근거

ORD 기록
ord-fc447e0cce384552b3ecf24a8b3c6750
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08389527B2

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