Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) → HCID 57813532, 화합물

HRID 564652노트

반응식

HRID 564652 반응식
[CH2:1]([N:3]1[C:7]2=[N:8][C:9]([CH2:32][CH3:33])=[C:10]([CH2:19][NH:20][C:21]([C:23]3[CH:24]=[C:25]([CH:29]=[CH:30][CH:31]=3)[C:26]([OH:28])=O)=[O:22])[C:11]([NH:12][CH:13]3[CH2:18][CH2:17][O:16][CH2:15][CH2:14]3)=[C:6]2[CH:5]=[N:4]1)[CH3:2].Cl.Cl.[CH3:36][N:37]1[CH:42]2[CH2:43][CH2:44][CH:38]1[CH2:39][CH:40]([CH2:45][C:46]1[CH:47]=[C:48]([C:52]3[CH:57]=[CH:56][CH:55]=[C:54]([CH2:58][NH2:59])[CH:53]=3)[CH:49]=[CH:50][CH:51]=1)[CH2:41]2.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CS(C)=O>[CH2:1]([N:3]1[C:7]2=[N:8][C:9]([CH2:32][CH3:33])=[C:10]([CH2:19][NH:20][C:21]([C:23]3[CH:31]=[CH:30][CH:29]=[C:25]([C:26]([NH:59][CH2:58][C:54]4[CH:53]=[C:52]([C:48]5[CH:49]=[CH:50][CH:51]=[C:46]([CH2:45][CH:40]6[CH2:39][CH:38]7[N:37]([CH3:36])[CH:42]([CH2:43][CH2:44]7)[CH2:41]6)[CH:47]=5)[CH:57]=[CH:56][CH:55]=4)=[O:28])[CH:24]=3)=[O:22])[C:11]([NH:12][CH:13]3[CH2:14][CH2:15][O:16][CH2:17][CH2:18]3)=[C:6]2[CH:5]=[N:4]1)[CH3:2]

참가 물질

5

반응물 3

HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 578132773-[({[1,6-Diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)carbonyl]benzoic AcidHCID 67006469HCID 67006469, 화합물

생성물 1

HCID 57813532HCID 57813532, 화합물수율 54.2%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of 3-[({[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)carbonyl]benzoic acid (0.045 g, 0.1 mmol) in DMSO (0.5 mL) was added 1-{3′-[(8-methyl-8-azabicyclo[3.2.1]oct-3-yl)methyl]-3-biphenylyl}methanamine dihydrochloride (0.047 g, 0.12 mmol), HBTU (0.054 g, 0.15 mmol), and TEA (0.042 mL, 0.3 mmol) and the reaction was stirred at room temperature for 16 h. The reaction mixture was purified using a Gilson HPLC (with 0.1% TFA), concentrated, basified with amino cartridge to afford 0.0409 g (52%) of the title compound. LC-MS m/z 754 (M+H)+.

후처리

  1. customThe reaction mixture was purified
  2. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ed244d292345429f8ca2d04ec40a19ca
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067408B2

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