Triethylamine → HCID 135546172, 화합물

HRID 2375116노트

반응식

HRID 2375116 반응식
[NH2:1][C:2]1[CH:3]=[C:4]2[C:14](=[O:15])[NH:13][N:12]=[CH:11][C:6]3=[CH:7][NH:8][C:9]([CH:10]=1)=[C:5]23.[CH2:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH2:19][CH2:18][N:17]1[CH2:26][C:27]([OH:29])=O.C(N([CH2:35][CH3:36])CC)C.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)[C:48]2N=C[CH:51]=[CH:52][C:47]=2N=N1>CN(C)C=O>[CH2:16]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH2:19][CH2:18][N:17]1[CH2:26][C:27]([NH:1][C:2]1[CH:3]=[C:4]2[C:14](=[O:15])[NH:13][N:12]=[CH:11][C:6]3=[C:7]([C:36]4[CH:35]=[CH:51][CH:52]=[CH:47][CH:48]=4)[NH:8][C:9]([CH:10]=1)=[C:5]23)=[O:29]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 1514441(3,4-Dihydro-1H-isoquinolin-2-yl)-acetic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 135774128HCID 135774128, 화합물

생성물 1

HCID 135546172HCID 135546172, 화합물수율 34%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In a manner analogous to that of Example 11, to a stirred solution of 8-amino-1,5-dihydro-6H-[1,2]diazepino[4,5,6-cd] indol-6-one in anhydrous N,N-dimethylformamide (6 mL) was added 3,4-dihydroisoquinolin-2(1H)-ylacetic acid (62 mg, 0.33 mmol) followed by triethylamine (0.14 mL, 0.98 mmol) and O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (372 mg, 0.98 mmol). The reaction was stirred at room temperature for 17 hours. After concentrating, water was added and the precipitated solid was collected by filtration. After preparative HPLC, the title compound (50 mg) was obtained as a yellow powder in 34% yield.

후처리

  1. concentrationAfter concentrating
  2. additionwater was added
  3. filtrationthe precipitated solid was collected by filtration

출처 및 근거

ORD 기록
ord-538e65681a324215b3aefc7aa9185eba
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07462713B2

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