Hydrochloric Acid → 1-(2-(1-(3,5-Dimethoxyphenyl)ethylamino)-4-(piperazin-1-yl)phenyl)-2,2,2-trifluoroethanone hydrochloride

HRID 1910530ノート

反応式

HRID 1910530 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]([NH:13][C:14]2[CH:15]=[C:16]([N:26]3[CH2:31][CH2:30][N:29](C(OC(C)(C)C)=O)[CH2:28][CH2:27]3)[CH:17]=[CH:18][C:19]=2[C:20](=[O:25])[C:21]([F:24])([F:23])[F:22])[CH3:12])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.[ClH:39]>ClCCl.CO.C(OCC)C>[ClH:39].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]([NH:13][C:14]2[CH:15]=[C:16]([N:26]3[CH2:27][CH2:28][NH:29][CH2:30][CH2:31]3)[CH:17]=[CH:18][C:19]=2[C:20](=[O:25])[C:21]([F:22])([F:24])[F:23])[CH3:12])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 58707263t-Butyl 4-(3-(1-(3,5-dimethoxyphenyl)ethylamino)-4-(2,2,2-trifluoroacetyl)phenyl)piperazine-1-carboxylate

生成物 1

HCID 671473501-(2-(1-(3,5-Dimethoxyphenyl)ethylamino)-4-(piperazin-1-yl)phenyl)-2,2,2-trifluoroethanone hydrochloride収率 97%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of t-butyl 4-(3-(1-(3,5-dimethoxyphenyl)ethylamino)-4-(2,2,2-trifluoroacetyl)phenyl)piperazine-1-carboxylate (231 mg, 0.43 mmol) in dichloromethane (2.0 mL) and methanol (0.5 mL) was added a saturated solution of HCl in diethyl ether (20 mL). The reaction mixture was stirred for 3 hours. The solvent was removed by rotary evaporation to afford the title compound (198 mg, 97% yield). 1H NMR (400 MHz, CD3OD): δ 7.62 (m, 1H), 6.52 (s, 2H), 6.36 (m, 2H), 5.49 (s, 1H), 4.66 (m, 1H), 3.57 (m, 2H), 3.50 (m, 2H), 3.21 (m, 4H), 1.58 (d, 3H); MS (ESI) m/z: Calculated for C22H27F3N3O3: 438.2; Observed: 439.5 (M++1) [corresponding to the free base].

後処理

  1. customThe solvent was removed by rotary evaporation

出典と根拠

ORDレコード
ord-1a57141b497c4e21ad87127c58da42f8
出典データセット
uspto-grants-2013_12
特許番号
US08604021B2

反応ノート

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