Acetonitrile → HCID 23141667、化合物

HRID 32160ノート

反応式

HRID 32160 の反応式
[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:14]=[CH:13][C:12]([N:15]3[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]3)=[C:11]([C:21]3[CH2:26][CH2:25][C:24]4([CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]4)[CH2:23][CH:22]=3)[CH:10]=2)[CH2:5][CH2:4]1.[CH3:32][O:33][CH2:34][CH2:35]Br.C(=O)([O-])[O-].[K+].[K+].C(#N)C>[Cl-].[Na+].O.C(OCC)(=O)C>[CH3:32][O:33][CH2:34][CH2:35][N:18]1[CH2:19][CH2:20][N:15]([C:12]2[CH:13]=[CH:14][C:9]([N:6]3[CH2:7][CH2:8][CH:3]([O:2][CH3:1])[CH2:4][CH2:5]3)=[CH:10][C:11]=2[C:21]2[CH2:26][CH2:25][C:24]3([CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)[CH2:23][CH:22]=2)[CH2:16][CH2:17]1

参加物

7

反応物 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 809722-Bromoethyl methyl etherHCID 231420141-[4-(4-Methoxypiperidin-1-yl)-2-spiro[5.5]undec-2-en-3-yl-phenyl]piperazine

生成物 1

HCID 23141667HCID 23141667、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒2 回HCID 57417360Sodium chloride; water溶媒

反応条件

温度
80 °C

実験手順

A mixture of 1-[4-(4-methoxypiperidin-1-yl)-2-spiro[5.5]undec-2-en-3-yl-phenyl]piperazine (20 mg, 0.0472 mmol) produced in Example (39e), 2-bromoethyl methyl ether (0.0049 mL, 0.0519 mmol), potassium carbonate (11.1 mg, 0.0803 mmol) and acetonitrile (1 mL) was stirred for 5 hours at an external temperature of 80° C. Ethyl acetate and brine were added to the reaction mixture and extraction was performed three times with ethyl acetate. The separated organic layers were concentrated. The resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 1-(2-methoxyethyl)-4-[4-(4-methoxypiperidin-1-yl)-2-spiro[5.5]undec-2-en-3-ylphenyl]piperazine.

後処理

  1. concentrationThe separated organic layers were concentrated
  2. customThe resultant residue was purified by NH silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-1e8ff9f29ad6468683b34d1fe9ea5440
出典データセット
uspto-grants-2008_09
特許番号
US07425554B2

反応ノート

読み込み中…