Ammonia → HCID 66628688, 화합물

HRID 2200990노트

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HRID 2200990 반응식
C[N:2](C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)CC)C.[C:32]([C:34]1[C@@H:39]([C:40]2[CH:45]=[CH:44][C:43]([C:46]#[N:47])=[CH:42][CH:41]=2)[N:38]2[N:48]=[C:49]([NH:51][CH2:52][C:53](O)=[O:54])[N:50]=[C:37]2[N:36]([C:56]2[CH:61]=[CH:60][CH:59]=[C:58]([C:62]([F:65])([F:64])[F:63])[CH:57]=2)[C:35]=1[CH3:66])#[N:33].N.O1CCOCC1>CN(C=O)C>[C:32]([C:34]1[C@@H:39]([C:40]2[CH:45]=[CH:44][C:43]([C:46]#[N:47])=[CH:42][CH:41]=2)[N:38]2[N:48]=[C:49]([NH:51][CH2:52][C:53]([NH2:2])=[O:54])[N:50]=[C:37]2[N:36]([C:56]2[CH:61]=[CH:60][CH:59]=[C:58]([C:62]([F:65])([F:63])[F:64])[CH:57]=2)[C:35]=1[CH3:66])#[N:33]

참가 물질

7

반응물 5

HCID 222AmmoniaHCID 8471TriethylamineHCID 312751,4-DioxaneHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 66628192HCID 66628192, 화합물

생성물 1

HCID 66628688HCID 66628688, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

Under an atmosphere of argon protective gas and at 0° C., HATU (25 mg, 66 μmol, 3 eq.) and triethylamine (11 mg, 110 μmol, 5 eq.) were added to a solution of N-{(7R)-6-cyano-7-(4-cyanophenyl)-5-methyl-4-[3-(trifluoromethyl)phenyl]-4,7-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-2-yl}glycine (10.5 mg, 22 μmol) in DMF (1 ml). After the reaction mixture has thawed to RT, it was once more cooled to 0° C., and a 0.5 M solution of ammonia in dioxane (0.44 ml, 219 μmol, 10 eq.) was then added. The mixture was stirred for 2 h, during which time it gradually warmed to RT. The reaction mixture was then concentrated under reduced pressure and the residue was purified by preparative HPLC (Kromasil C18 column, 50×20 mm; mobile phase: acetonitrile-water-0.1% TFA). After lyophilization, the product was obtained as a solid (9.2 mg, 88% of theory).

후처리

  1. customhas thawed to RT
  2. temperaturegradually warmed to RT
  3. concentrationThe reaction mixture was then concentrated under reduced pressure
  4. customthe residue was purified by preparative HPLC (Kromasil C18 column, 50×20 mm; mobile phase: acetonitrile-water-0.1% TFA)
  5. customAfter lyophilization, the product was obtained as a solid (9.2 mg, 88% of theory)

출처 및 근거

ORD 기록
ord-d43bbed047ad498ebc245db62556e6a1
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359362B2

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