Trifluoroacetic acid → (3-Chloro-4-(4-methylpiperazin-1-yl)phenyl)methanamine

HRID 1819680

反応式

HRID 1819680 の反応式
ClC1C=C(C=C(Cl)C=1N)CN.[Cl:12][C:13]1[CH:14]=[C:15]([CH:25]=[CH:26][C:27]=1[N:28]1[CH2:33][CH2:32][N:31]([CH3:34])[CH2:30][CH2:29]1)[CH2:16][NH:17]C(=O)OC(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[Cl:12][C:13]1[CH:14]=[C:15]([CH2:16][NH2:17])[CH:25]=[CH:26][C:27]=1[N:28]1[CH2:29][CH2:30][N:31]([CH3:34])[CH2:32][CH2:33]1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 189757634-Amino-3,5-dichlorobenzylamineHCID 69058940Tert-butyl 3-chloro-4-(4-methylpiperazin-1-yl)benzylcarbamate

生成物 1

HCID 57887239(3-Chloro-4-(4-methylpiperazin-1-yl)phenyl)methanamine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Step F (3): To a solution of tert-butyl 3-chloro-4-(4-methylpiperazin-1-yl)benzylcarbamate (36 mg, 0.1 mmol) from step F (2) in CH2Cl2 (0.5 mL) was added TFA (0.5 mmol). The mixture was stirred at rt for 2 h, and then the mixture was concentrated to give the title compound which was used without further purification. 1H-NMR (500 MHz, CD3OD) δ 7.59 (s, 1 H), 7.43 (d, J=8.24 Hz, 1 H), 7.27 (d, J=8.24 Hz, 1 H), 4.10 (s, 2 H), 3.60-3.70 (m, 2 H), 3.50-3.59 (m, 2 H), 3.29-3.42 (m, 2 H), 3.10-3.22 (m, 2 H), 2.98 (s, 3 H).

後処理

  1. concentrationthe mixture was concentrated

出典と根拠

ORDレコード
ord-7dbeb1c906f549c6a258bff6663384d0
出典データセット
uspto-grants-2009_10
特許番号
US07601751B2

関連ノート

読み込み中…