Triethylamine → HCID 135546172、化合物

HRID 2375116ノート

反応式

HRID 2375116 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.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]

参加物

6

反応物 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、化合物

生成物 1

HCID 135546172HCID 135546172、化合物収率 34%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

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 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.

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-538e65681a324215b3aefc7aa9185eba
出典データセット
uspto-grants-2008_12
特許番号
US07462713B2

反応ノート

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