Diisopropylethylamine → HCID 178502366、化合物

HRID 1800802ノート

反応式

HRID 1800802 の反応式
[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]

参加物

6

反応物 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、化合物

生成物 1

HCID 178502366HCID 178502366、化合物収率 58.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-884f824a59ee429bad0aaf74eec09105
出典データセット
uspto-grants-2013_01
特許番号
US08344155B2

反応ノート

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