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Sodium Hydroxide → HCID 57731467、化合物

HRID 2234693
ノート
印刷プレビュー

反応式

HRID 2234693 の反応式
F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2[N:13]=[CH:14][CH:15]=[CH:16][C:11]=2N=N1.[CH3:25][O:26][C:27]([NH:29][C:30]1[CH:38]=[CH:37][C:36]([C:39]2[CH:40]=[C:41]3[C:47]([C:48]4[CH:53]=[CH:52][CH:51]=[CH:50][C:49]=4[O:54][CH3:55])=[CH:46][N:45](S(C4C=CC(C)=CC=4)(=O)=O)[C:42]3=[N:43][CH:44]=2)=[CH:35][C:31]=1[C:32]([OH:34])=O)=[O:28].N1CCCC1.C(N(C(C)C)CC)(C)C.[OH-].[Na+]>CN(C)C=O.C(O)(=O)C.CO>[CH3:25][O:26][C:27](=[O:28])[NH:29][C:30]1[CH:38]=[CH:37][C:36]([C:39]2[CH:40]=[C:41]3[C:47]([C:48]4[CH:53]=[CH:52][CH:51]=[CH:50][C:49]=4[O:54][CH3:55])=[CH:46][NH:45][C:42]3=[N:43][CH:44]=2)=[CH:35][C:31]=1[C:32]([N:13]1[CH2:14][CH2:15][CH2:16][CH2:11]1)=[O:34]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 14798Sodium HydroxideHCID 31268PyrrolidineHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 57731438HCID 57731438、化合物

生成物 1

HCID 57731467
HCID 57731467、化合物
収率 36%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

O-(7-Azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (49.9 mg, 0.13 mmol) was added to a solution of 2-methoxycarbonylamino-5-[3-(2-methoxy-phenyl)-1-(toluene-4-sulfonyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]-benzoic acid (75 mg, 0.13 mmol), pyrrolidine (9.33, 0.13 mmol) and di-iso-propyl ethyl amine (51 mg, 0.39 mmol) in N,N-Dimethylformamide (1 ml). The reaction was stirred at room temperature for 1 hour, then methanol (2 ml) was added followed by aqueous sodium hydroxide (0.2 ml) and the reaction was stirred at room temperature for 16 hours. This solution was then neutralized with acetic acid and the compound was purified by preparative mass-triggered reverse-phase HPLC chromatography to give [4-[3-(2-methoxy-phenyl)-1H-pyrrolo[2,3-b]pyridin-5-yl]-2-(pyrrolidine-1-carbonyl)-phenyl]-carbamic acid methyl ester as a white solid.). 1H NMR (500 MHz, DMSO-d6) δ 1.81 (p, J=6 Hz 1H); 1.87 (p, J=6 Hz 1H); 3.41 (t, J=6 Hz 1H); 3.48 (t, J=6 Hz 1H); 3.65 (s, 3H); 3.81 (s, 3H); 7.04 (t, J=8 Hz 1H) 7.13 (d, J=8 Hz 1H); 7.29 (t, J=8 Hz, 1H); 7.60 (d, J=8 Hz 1H); 7.75 (m, 4H); 8.17 (s, 1H); 8.55 (s, 1H); 9.23 (s, br, 1H); 11.95 (s, br, 1H) (21.8 mg, 36% yield MS: m/z 471.5 (M+H+).

後処理

  1. stirringthe reaction was stirred at room temperature for 16 hours
  2. customthe compound was purified by preparative mass-triggered reverse-phase HPLC chromatography

出典と根拠

ORDレコード
ord-e2802e9f5486400ab2f53459286a8507
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709645B2

反応ノート

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