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Tetrahydrofuran → HCID 178521456、化合物

HRID 1047363
ノート
印刷プレビュー

反応式

HRID 1047363 の反応式
Cl[CH2:2][C:3]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)=[O:4].[N+:21]([C:24]1[CH:29]=[CH:28][C:27]([NH:30][C@H:31]2[CH2:36][CH2:35][C@H:34]([OH:37])[CH2:33][CH2:32]2)=[CH:26][C:25]=1[C:38]([F:41])([F:40])[F:39])([O-:23])=[O:22].[H-].[Na+].O1CCCC1>ClCCl.CN(C)C=O>[N+:21]([C:24]1[CH:29]=[CH:28][C:27]([NH:30][C@H:31]2[CH2:36][CH2:35][C@H:34]([O:37][CH2:2][C:3]([N:5]3[CH2:10][CH2:9][N:8]([C:11]4[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][CH:12]=4)[CH2:7][CH2:6]3)=[O:4])[CH2:33][CH2:32]2)=[CH:26][C:25]=1[C:38]([F:39])([F:40])[F:41])([O-:23])=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 581182122-Chloro-1-[4-[4-(trifluoromethyl)phenyl]piperazin-1-yl]ethan-1-oneHCID 178526690HCID 178526690、化合物

生成物 1

HCID 178521456HCID 178521456、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒

実験手順

2-Chloro-1-[4-(4-trifluoromethyl-phenyl)-piperazin-1-yl]-ethanone (26 mg, 0.09 mmol, prepared in accordance with Example 4), trans-4-(4-nitro-3-trifluoromethyl-phenylamino)-cyclohexanol (26 mg, 0.09 mmol, prepare in accordance with Example 5), and sodium hydride (10 mg, 60% in oil, 0.26 mmol) were placed under an inert atmosphere. Tetrahydrofuran (1 mL) was added under stirring. Next, dimethylformamide (300 μL) was added under stirring. The resulting mixture was stirred for 40 min at room temperature and then diluted with dichloromethane (5 mL). The mixture was washed with water (5 mL) and then washed with saturated aqueous sodium hydrogencarbonate (5 mL). The organic phase was collected, dried over magnesium sulfate, filtered, and concentrated under vacuum. The crude product was purified by preparative HPLC. Following lyophilization of the fractions of interest, the desired product was isolated as a yellow solid (21 mg, 43% yield). The structure was confirmed using Protocol II-A. Calculated mass=575; observed mass=575; HPLC retention time=4.51 min.

後処理

  1. stirringunder stirring
  2. stirringThe resulting mixture was stirred for 40 min at room temperature
  3. washThe mixture was washed with water (5 mL)
  4. washwashed with saturated aqueous sodium hydrogencarbonate (5 mL)
  5. customThe organic phase was collected
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum
  9. customThe crude product was purified by preparative HPLC

出典と根拠

ORDレコード
ord-68ca62a907c04bdabbb9771cf8a7c76a
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569495B2

反応ノート

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