Dimethylformamide → HCID 135546172, 화합물

HRID 1064197노트

반응식

HRID 1064197 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.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)[C:41]2N=[CH:43][CH:44]=[CH:45][C:40]=2N=N1.[CH3:54]N(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:41]4[CH:54]=[CH:43][CH:44]=[CH:45][CH:40]=4)[NH:8][C:9]([CH:10]=1)=[C:5]23)=[O:29]

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 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%

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 tiethylamine (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-866b4f4c059348dfa66b0035ea2d293d
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06967198B2

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