1-Methoxy-2-propanol → HCID 66711135、化合物

HRID 1261993ノート

反応式

HRID 1261993 の反応式
CS([C:4]1[N:9]=[CH:8][C:7]2=[CH:10][CH:11]=[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[O:19][CH3:20])[N:6]2[N:5]=1)=O.C(N(CC)C(C)C)(C)C.[N:30]1([CH:36]2[CH2:41][CH2:40][N:39]([C:42]3[CH:47]=[CH:46][C:45]([NH2:48])=[CH:44][CH:43]=3)[CH2:38][CH2:37]2)[CH2:35][CH2:34][O:33][CH2:32][CH2:31]1.COCC(O)C>>[CH3:20][O:19][C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[C:12]1[N:6]2[C:7]([CH:8]=[N:9][C:4]([NH:48][C:45]3[CH:46]=[CH:47][C:42]([N:39]4[CH2:38][CH2:37][CH:36]([N:30]5[CH2:35][CH2:34][O:33][CH2:32][CH2:31]5)[CH2:41][CH2:40]4)=[CH:43][CH:44]=3)=[N:5]2)=[CH:10][CH:11]=1

参加物

5

反応物 4

HCID 79001-Methoxy-2-propanolHCID 81531DiisopropylethylamineHCID 210915834-(4-Morpholinopiperidin-1-yl)anilineHCID 667107912-Methanesulfinyl-7-(2-methoxy-phenyl)-pyrrolo[2,1-f][1,2,4]triazine

生成物 1

HCID 66711135HCID 66711135、化合物収率 21%

実験手順

2-Methanesulfinyl-7-(2-methoxy-phenyl)-pyrrolo[2,1-f][1,2,4]triazine (125.0 mg, 0.0004350 mol), N,N-Diisopropylethylamine (0.114 mL, 0.000652 mol) and 4-(4-Morpholin-4-yl-piperidin-1-yl)-phenylamine (0.227 g, 0.000870 mol) were dissolved in 1-Methoxy-2-propanol (1.2 mL, 0.013 mol) and The reaction was irradiated at 300 watts, 180° C. for 40 minutes or until HPLC showed consumption of starting material. The reaction mixture was then reduced en vacuo and the product was isolated and purified by Gilson prep HPLC to afford 44.36 mg of [7-(2-Methoxy-phenyl)-pyrrolo[2,1-f][1,2,4]triazin-2-yl]-[4-(4-morpholin-4-yl-piperidin-1-yl)-phenyl]-amine as a lyophilized powder. (M+H)=485.8. 1H NMR (400 MHz, DMSO, d6) δ 9.20 (s, 1H), 8.91 (s, 1H), 7.82 (dd, 1H, J=1.56, 6.16 Hz), 7.60 (d, 2H, J=9.01 Hz), 7.45 (m, 1H), 7.21 (d, 1H, J=8.17 Hz), 7.12 (t, 1H, J=7.28 Hz), 6.90 (m, 4H), 4.02 (m, 2H), 3.80 (s, 3H), 3.50 (m, 5H), 3.35 (m, 2H), 3.24 (m, 2H), 2.71 (m, 2H), 2.12 (m, 2H), 1.70 (m, 2H).

後処理

  1. customThe reaction was irradiated at 300 watts, 180° C. for 40 minutes or until HPLC
  2. customconsumption of starting material
  3. customthe product was isolated
  4. custompurified by Gilson prep HPLC

出典と根拠

ORDレコード
ord-7e65ba4fb715482f9f1bfdb4b5dcd283
出典データセット
uspto-grants-2013_06
特許番号
US08471005B2

反応ノート

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