Triethylamine → HCID 178476968, 화합물

HRID 1525230노트

반응식

HRID 1525230 반응식
[OH:1][C:2]1[C:7]([C:8]([OH:10])=O)=[CH:6][N:5]=[C:4]([N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)[N:3]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(CC)CC.[NH2:47][CH:48]([C:63]1[CH:68]=[CH:67][CH:66]=[CH:65][CH:64]=1)[C:49]1[CH:54]=[CH:53][C:52]([P:55](=[O:62])([O:59][CH2:60][CH3:61])[O:56][CH2:57][CH3:58])=[CH:51][CH:50]=1>CC#N>[OH:1][C:2]1[C:7]([C:8]([NH:47][CH:48]([C:63]2[CH:64]=[CH:65][CH:66]=[CH:67][CH:68]=2)[C:49]2[CH:54]=[CH:53][C:52]([P:55](=[O:62])([O:56][CH2:57][CH3:58])[O:59][CH2:60][CH3:61])=[CH:51][CH:50]=2)=[O:10])=[CH:6][N:5]=[C:4]([N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)[N:3]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 89462707Diethyl 4-(amino(phenyl)methyl)phenylphosphonate2회HCID 178524762HCID 178524762, 화합물2회

생성물 1

HCID 178476968HCID 178476968, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 4-hydroxy-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid, 8-b, (309 mg, 1.5 mmol) in MeCN (10 ml) were added HATU (599 mg, 1.58 mmol), Et3N (159 mg, 1.58 mmol) and diethyl 4-(amino(phenyl)methyl)phenylphosphonate, 2-c, (479 mg, 1.5 mmol). The resulting mixture was stirred at room temperature for 2 hours. Then it was concentrated under vacuum and the residue was taken into ethyl acetate followed by washing with sat. NH4Cl. The organic layer was dried over sodium sulfate and concentrated under vacuum. The residue was purified by prep-HPLC to provide the product, 8-1, (150 mg, 20%). 1H NMR (CD3OD, 300 MHz,): δ 10.39 (br, 1H), 8.56 (s, 1H), 8.47 (m, 1H), 7.81 (m, 1H), 7.62 (m, 2H), 7.40 (m, 2H), 7.25 (m, 5H), 6.54 (m, 1H), 6.26 (m, 1H), 3.96 (m, 4H), 1.18 (m, 6H).

후처리

  1. concentrationThen it was concentrated under vacuum
  2. washby washing with sat. NH4Cl
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. concentrationconcentrated under vacuum
  5. customThe residue was purified by prep-HPLC
  6. customto provide the product, 8-1, (150 mg, 20%)

출처 및 근거

ORD 기록
ord-7ad4f8e4765e4b588fd23f8145b8b77f
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09079930B2

반응 노트

불러오는 중…