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Triethylamine → 4-(azetidine-1-carbonyl)-1-methyl-N-(6-methyl-2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-1H-pyrazole-5-carboxamide

HRID 1802160
ノート
印刷プレビュー

反応式

HRID 1802160 の反応式
Cl.[CH3:2][C:3]1[C:4]([NH2:18])=[CH:5][C:6]2[N:7]([N:9]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[N:11]=2)[CH:8]=1.C(N(CC)CC)C.C[Al](C)C.[N:30]1([C:34]([C:36]2[CH:37]=[N:38][N:39]([CH3:46])[C:40]=2[C:41](OCC)=[O:42])=[O:35])[CH2:33][CH2:32][CH2:31]1.C(N(C(C)C)C(C)C)C>O1CCOCC1>[N:30]1([C:34]([C:36]2[CH:37]=[N:38][N:39]([CH3:46])[C:40]=2[C:41]([NH:18][C:4]2[C:3]([CH3:2])=[CH:8][N:7]3[N:9]=[C:10]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)[N:11]=[C:6]3[CH:5]=2)=[O:42])=[O:35])[CH2:31][CH2:32][CH2:33]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8471TriethylamineHCID 81531DiisopropylethylamineHCID 16682925Trimethylaluminum2 回HCID 67041800ethyl 4-(azetidine-1-carbonyl)-1-methyl-1H-pyrazole-5-carboxylateHCID 677760476-Methyl-2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-amine hydrochloride

生成物 1

HCID 57377305
4-(azetidine-1-carbonyl)-1-methyl-N-(6-methyl-2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-1H-pyrazole-5-carboxamide
収率 24.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
25 °C

実験手順

To an argon purged solution of 6-methyl-2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-amine hydrochloride (147 mg, 564 μmol) and triethylamine (78.6 μl, 564 μmol) in dioxane (8 ml) is added trimethylaluminum (2M solution in toluene, 705 μl, 1.41 mmol). The resulting mixture is stirred for 1 hour at 25° C., then ethyl 4-(azetidine-1-carbonyl)-1-methyl-1H-pyrazole-5-carboxylate (134 mg, 564 μmol) is added; the mixture is heated to 100° C. and stirred for 18 hours. As no conversion is detected N-ethyl diisopropylamine (246 μl, 1.41 mmol) and another portion of trimethylaluminum (2M solution in toluene, 705 μl, 1.41 mmol) are added, the mixture is stirred for 1 hours at 25° C. and then for further 20 hours at 100° C. The crude material is loaded on silica and purified by flash chromatography on a 20 g silica column using heptane/ethyl acetate 10-100% as eluent affording 4-(azetidine-1-carbonyl)-1-methyl-N-(6-methyl-2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-yl)-1H-pyrazole-5-carboxamide (57 mg, 24.3%) as a light yellow solid. mp.: 226-8° C. MS: m/z=416.2 (M+H+).

後処理

  1. temperaturethe mixture is heated to 100° C.
  2. stirringstirred for 18 hours
  3. stirringthe mixture is stirred for 1 hours at 25° C.
  4. waitfor further 20 hours at 100° C
  5. custompurified by flash chromatography on a 20 g silica column

出典と根拠

ORDレコード
ord-129b1e3a7d944007bcbab532fd6e8c26
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08349824B2

反応ノート

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