p-Toluenesulfonic acid → HCID 66660252、化合物

HRID 1383842ノート

反応式

HRID 1383842 の反応式
Cl[C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][C:7]=1[C:8]1[O:9][CH:10]=[CH:11][CH:12]=1.Cl.C([N:17]([CH2:20][CH3:21])CC)C.[C:22]1(C)C=[CH:26][C:25](S(O)(=O)=O)=[CH:24][CH:23]=1.[CH3:33][N:34]1[CH:38]=[N:37][C:36]([CH2:39][OH:40])=[N:35]1.[N:41]1C=CC=CC=1CO>C(N(CC)CC)C>[O:9]1[CH:10]=[CH:11][CH:12]=[C:8]1[C:7]1[C:2]([O:40][CH2:39][C:36]2[N:37]=[CH:38][N:34]([CH3:33])[N:35]=2)=[N:3][N:4]2[C:20]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[N:17][N:41]=[C:5]2[CH:6]=1

参加物

7

反応物 5

HCID 6101p-Toluenesulfonic acidHCID 11130Triethylamine hydrochlorideHCID 11474PiconolHCID 10351670(1-Methyl-1H-1,2,4-triazol-3-yl)methanolHCID 21187529Pyridazine, 3,6-dichloro-4-(2-furanyl)-

生成物 1

HCID 66660252HCID 66660252、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

This compound was prepared from 3,6-dichloro-4-(furan-2-yl)-pyridazine (Example 140 part a) using the procedures described in Example 16 Steps b) and c) except 1.1 equivalents of triethylamine hydrochloride was used in Step b) instead of 1.1 equivalents of p-toluenesulphonic acid and triethylamine, and (1-methyl-1 H-1,2,4-triazol-3yl)methanol (Example 65) was used in Step c) instead of 2-pyridylcarbinol. Data for the title compound: m.p. 257-259° C. (DMF). 1H NMR (360 MHz, d6-DMSO) 3.91 (3 H s), 5.63 (2 H, s), 6.74 (1 H, dd, J=4 and 2 Hz), 7.33 (1 H, d, J=4 Hz), 7.54-7.65 (3 H, m), 7.99 (1 H, d, J=2 Hz), 8.44 (1 H, s), 8.46 (2 H, d, J=7 Hz), 8.57 (1 H, s). MS (ES+) 374 [MH]+. Anal. Found C, 60.68; H 4.11; N, 25.82. C19H15N7O2. 0.15 H2O requires C, 60.68; H, 4.10; N, 26.07%.

出典と根拠

ORDレコード
ord-d4036760b4484aee8ec56abe6eb4d119
出典データセット
uspto-grants-2001_07
特許番号
US06255305B1

反応ノート

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