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Tert-butyl (2S)-4-{4-[({4-[(4-chlorophenyl)sulfonyl]cyclohexyl}carbonyl)(methyl)amino]-2-methylbenzyl}-2-methylpiperazine-1-carboxylate → 4-[(4-Chlorophenyl)sulfonyl]-N-methyl-N-(3-methyl-4-{[(3S)-3-methylpiperazin-1-yl]methyl}phenyl)cyclohexanecarboxamide

HRID 2170290
ノート
印刷プレビュー

反応式

HRID 2170290 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH:11]2[CH2:16][CH2:15][CH:14]([C:17]([N:19]([CH3:42])[C:20]3[CH:40]=[CH:39][C:23]([CH2:24][N:25]4[CH2:30][CH2:29][N:28](C(OC(C)(C)C)=O)[C@@H:27]([CH3:38])[CH2:26]4)=[C:22]([CH3:41])[CH:21]=3)=[O:18])[CH2:13][CH2:12]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1>ClCCl.FC(F)(F)C(O)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH:11]2[CH2:16][CH2:15][CH:14]([C:17]([N:19]([CH3:42])[C:20]3[CH:40]=[CH:39][C:23]([CH2:24][N:25]4[CH2:30][CH2:29][NH:28][C@@H:27]([CH3:38])[CH2:26]4)=[C:22]([CH3:41])[CH:21]=3)=[O:18])[CH2:13][CH2:12]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 86700730Tert-butyl (2S)-4-{4-[({4-[(4-chlorophenyl)sulfonyl]cyclohexyl}carbonyl)(methyl)amino]-2-methylbenzyl}-2-methylpiperazine-1-carboxylate2 回

生成物 1

HCID 867007314-[(4-Chlorophenyl)sulfonyl]-N-methyl-N-(3-methyl-4-{[(3S)-3-methylpiperazin-1-yl]methyl}phenyl)cyclohexanecarboxamide収率 100%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid
溶媒

実験手順

To a solution of tert-butyl (2S)-4-{4-[({4-[(4-chlorophenyl)sulfonyl]cyclohexyl}carbonyl)(methyl)amino]-2-methylbenzyl}-2-methylpiperazine-1-carboxylate (80.2 mg, 0.13 mmol) synthesized in (10D) in dichloromethane (1 mL), trifluoroacetic acid (10 mL) was added at room temperature, and the resulting mixture was stirred at room temperature for 30 minutes. The solvent was distilled off under reduced pressure, and the obtained residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=100:0 to 90:10 (v/v)), whereby the title compound was obtained as an oil (50.1 mg, yield: 100%).

後処理

  1. additionwas added at room temperature
  2. distillationThe solvent was distilled off under reduced pressure
  3. customthe obtained residue was purified by NH silica gel column chromatography (ethyl acetate:methanol=100:0 to 90:10 (v/v)), whereby the title compound

出典と根拠

ORDレコード
ord-2db375145c1a425a94bb1aad25a4346f
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051255B2

反応ノート

読み込み中…

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