Diisopropylethylamine → HCID 66711542、化合物

HRID 1261934ノート

反応式

HRID 1261934 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[N:16]3[C:11]([CH:12]=[N:13][C:14](S(C)=O)=[N:15]3)=[CH:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1.C(N(CC)C(C)C)(C)C.[N:29]1([C:34]2[CH:39]=[CH:38][C:37]([NH2:40])=[CH:36][CH:35]=2)[CH2:33][CH2:32][CH2:31][CH2:30]1>COCCO>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[N:16]3[C:11]([CH:12]=[N:13][C:14]([NH:40][C:37]4[CH:36]=[CH:35][C:34]([N:29]5[CH2:33][CH2:32][CH2:31][CH2:30]5)=[CH:39][CH:38]=4)=[N:15]3)=[CH:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 8088414-(Pyrrolidin-1-yl)anilineHCID 66710773HCID 66710773、化合物

生成物 1

HCID 66711542HCID 66711542、化合物収率 16.1%

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

実験手順

7-(3-Chloro-phenyl)-2-methanesulfinyl-pyrrolo[2,1-f][1,2,4]triazine (125.0 mg, 0.0004284 mol), N,N-Diisopropylethylamine (0.112 mL, 0.000643 mol) and 4-Pyrrolidin-1-yl-phenylamine (139 mg, 0.000857 mol) were dissolved in 2-Methoxyethanol (3.01 mL) and The reaction was microwaved on 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 26.91 mg of [7-(3-Chloro-phenyl)-pyrrolo[2,1-f][1,2,4]triazin-2-yl]-(4-pyrrolidin-1-yl-phenyl)-amine as a lyophilized powder. (M+H)=390.09. 1H NMR (400 MHz, CDCl3) δ 9.63 (s, 1H), 8.63 (s, 1H), 8.32 (s, 1H), 7.84 (m, 1H), 7.76 (d, 2H, J=8.93 Hz), 7.48 (m, 2H), 7.34 (d, 2H, J=8.93 Hz), 7.21 (m, 1H), 7.18 (m, 1H), 3.66 (m, 4H), 2.25 (m, 4H).

後処理

  1. customThe reaction was microwaved on 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-83f5d40d05674ea18ebf907a9b26c4e6
出典データセット
uspto-grants-2013_06
特許番号
US08471005B2

反応ノート

読み込み中…