1-Methylpiperazine → HCID 178481075, 화합물

HRID 1620666노트

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HRID 1620666 반응식
Cl.[F:2][C:3]([F:34])([F:33])[C:4]1[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[CH:25][C:5]=1[CH2:6][N:7]1[CH2:12][CH2:11][CH:10](/[CH:13]=[C:14]2/[C:15]([NH:20]CC(O)=O)=[N:16][C:17](=[O:19])[S:18]/2)[CH2:9][CH2:8]1.[CH2:35]([N:37]([CH:41]([CH3:43])C)[CH:38]([CH3:40])C)[CH3:36].C[N:45]1[CH2:50]CNCC1.F[P-](F)(F)(F)(F)F.N1([O:67]C(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1>CN(C=O)C.O>[F:2][C:3]([F:34])([F:33])[C:4]1[CH:28]=[C:27]([C:29]([F:31])([F:32])[F:30])[CH:26]=[CH:25][C:5]=1[CH2:6][N:7]1[CH2:8][CH2:9][CH:10](/[CH:13]=[C:14]2/[C:15]([NH:20][CH2:43][C:41]([N:37]3[CH2:35][CH2:36][N:45]([CH3:50])[CH2:40][CH2:38]3)=[O:67])=[N:16][C:17](=[O:19])[S:18]/2)[CH2:11][CH2:12]1

참가 물질

7

반응물 4

HCID 531671-MethylpiperazineHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 178479765HCID 178479765, 화합물

생성물 1

HCID 178481075HCID 178481075, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of N-[(5Z)-5-({1-[2,4-bis(trifluoromethyl)benzyl]piperidin-4-yl}methylidene)-2-oxo-2,5-dihydro-1,3-thiazol-4-yl]glycine hydrochloride (500 mg), N-ethyl-N-(1-methylethyl)propan-2-amine (0.33 mL) and 1-methylpiperazine (0.11 mL) in DMF (5 mL) was added O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (429 mg), and the mixture was stirred at so room temperature for 2 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate), and the solid was recrystallized from diisopropyl ether/heptane to give the title compound (85 mg).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate)
  6. customthe solid was recrystallized from diisopropyl ether/heptane

출처 및 근거

ORD 기록
ord-09a39b1f56884e898b2be890905f1202
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772277B2

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