Dimethylformamide → HCID 135546172、化合物

HRID 1064197ノート

反応式

HRID 1064197 の反応式
[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]

参加物

5

反応物 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、化合物

生成物 1

HCID 135546172HCID 135546172、化合物収率 34%

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-866b4f4c059348dfa66b0035ea2d293d
出典データセット
uspto-grants-2005_11
特許番号
US06967198B2

反応ノート

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