Diisopropylethylamine → HCID 178502366, 화합물

HRID 1800802노트

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HRID 1800802 반응식
[CH3:1][O:2][C:3]([NH:5][C@H:6]([C:10]([N:12]1[C:16]2([CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)[CH2:15][CH2:14][CH:13]1C(O)=O)=[O:11])[CH:7]([CH3:9])[CH3:8])=[O:4].CC(C)[C@H](NC(OC)=O)C(N1C([C:45]([NH:47][CH2:48][C:49]([C:51]2[CH:56]=[CH:55][C:54]([C:57]3[CH:62]=[CH:61][C:60]([C:63]4[N:64]=[C:65]([C@@H:68]5[CH2:72][CH2:71][CH2:70][N:69]5[C:73](=[O:83])[C@@H:74]([NH:78][C:79]([O:81][CH3:82])=[O:80])[CH:75]([CH3:77])[CH3:76])[NH:66][CH:67]=4)=[CH:59][CH:58]=3)=[CH:53][CH:52]=2)=[O:50])=[O:46])CC2(CN(C(OC(C)(C)C)=O)C2)C1)=O.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>ClCCl>[CH3:76][CH:75]([CH3:77])[C@H:74]([NH:78][C:79](=[O:80])[O:81][CH3:82])[C:73]([N:69]1[CH2:70][CH2:71][CH2:72][C@H:68]1[C:65]1[NH:66][CH:67]=[C:63]([C:60]2[CH:59]=[CH:58][C:57]([C:54]3[CH:55]=[CH:56][C:51]([C:49](=[O:50])[CH2:48][NH:47][C:45]([CH:13]4[CH2:14][CH2:15][C:16]5([CH2:21][CH2:20][O:19][CH2:18][CH2:17]5)[N:12]4[C:10](=[O:11])[C@@H:6]([NH:5][C:3]([O:2][CH3:1])=[O:4])[CH:7]([CH3:9])[CH3:8])=[O:46])=[CH:52][CH:53]=3)=[CH:62][CH:61]=2)[N:64]=1)=[O:83]

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 583130871-{N-[(methyloxy)carbonyl]-L-valyl}-8-oxa-1-azaspiro[4.5]decane-2-carboxylic acidHCID 178502284HCID 178502284, 화합물

생성물 1

HCID 178502366HCID 178502366, 화합물수율 58.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-{N-[(methyloxy)carbonyl]-L-valyl}-8-oxa-1-azaspiro[4.5]decane-2-carboxylic acid (168) (52 mg, 1.5 mmol) and methyl {(1S)-1-[((2S)-2-{4-[4′-(aminoacetyl)-4-biphenylyl]-1H-imidazol-2-yl}-pyrrolidinyl)carbonyl]-2-methylpropyl}carbamate dihydrochloride (1) (88 mg, 0.15 mmol) and HATU (58 mg, 0.15 mmol) in anhydrous dichloromethane (1.2 mL) was added Hunig's base (0.12 mL, 0.68 mmol) and the reaction stirred at room temperature for 1 h. The reaction was concentrated in vacuo and purified by HPLC eluting with 10-90% water/acetonitrile/0.2% NH4OH to afford the title compound as an off-white solid (73 mg, 58% yield).

후처리

  1. concentrationThe reaction was concentrated in vacuo
  2. custompurified by HPLC
  3. washeluting with 10-90% water/acetonitrile/0.2% NH4OH

출처 및 근거

ORD 기록
ord-884f824a59ee429bad0aaf74eec09105
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08344155B2

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