Chloride → [3-Methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-(8-phenyl-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl)-amine hydrochloride

HRID 2076038ノート

反応式

HRID 2076038 の反応式
C(OC([N:8]1[CH2:32][CH:31]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[C:11]2[N:12]=[C:13]([NH:16][C:17]3[CH:22]=[CH:21][C:20]([N:23]4[CH:27]=[C:26]([CH3:28])[N:25]=[CH:24]4)=[C:19]([O:29][CH3:30])[CH:18]=3)[N:14]=[CH:15][C:10]=2[CH2:9]1)=O)(C)(C)C.[Cl-:39]>ClCCl.C(OCC)C>[ClH:39].[CH3:30][O:29][C:19]1[CH:18]=[C:17]([NH:16][C:13]2[N:14]=[CH:15][C:10]3[CH2:9][NH:8][CH2:32][CH:31]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)[C:11]=3[N:12]=2)[CH:22]=[CH:21][C:20]=1[N:23]1[CH:27]=[C:26]([CH3:28])[N:25]=[CH:24]1

参加物

5

反応物 2

HCID 312ChlorideHCID 441941562-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenylamino]-8-phenyl-7,8-dihydro-5H-pyrido[4,3-d]pyrimidine-6-carboxylic acid tert.-butyl ester

生成物 1

HCID 44194157[3-Methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-(8-phenyl-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl)-amine hydrochloride収率 100%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenylamino]-8-phenyl-7,8-dihydro-5H-pyrido[4,3-d]pyrimidine-6-carboxylic acid tert.-butyl ester (75 mg, 0.15 mmol) in dichloromethane (1.5 mL) was added at 0° C. 2M hydrogene chloride (0.73 mL) in diethyl ether. The reaction was stirred at room temperature over night. The solvent was evaporated under reduced pressure to yield the title compound (70 mg, 100%) as a yellow solid. MS ISP (m/e): 413.4 (100) [(M+H)+]. 1H NMR (DMSO-D6, 300 MHz): δ (ppm)=10.01 (m, 2H), 9.23 (s, 1H), 8.57 (s, 1H), 7.71 (s, 1H), 7.59 (s, 1H), 7.26-7.38 (m, 6H), 7.15 (d, 1H), 4.56 (dd, 1H), 4.37 (m, 2H), 3.64 (m, 1H), 3.42 (m, 1H), 3.38 (s, 3H), 2.32 (s, 3H).

後処理

  1. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-b9fe06ce9e744f31a31a703190f8d252
出典データセット
uspto-grants-2011_04
特許番号
US07923450B2

反応ノート

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